1、 g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58spectroscopyICS 59.080.01Determination of metals in textiles Part 2: Analysis by atomic emission BR
2、ITISH STANDARDBS 6810-2:2005BS 6810-2:2005This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 October 2005 BSI 31 October 2005The following BSI references relate to the work on this British Standard:Committee reference TCI/80Draft for comment
3、05/30091543 DCISBN 0 580 15878 0British Textile Technology GroupCo-operative UnionDefence Procurement AgencyLGCSATRA Technology CentreSociety of Dyers and ColouristsUK Cleaning Products Industry AssociationUK Textile Laboratory ForumWoolmark CompanyCo-opted membersAmendments issued since publication
4、Amd. No. Date CommentsCommittees responsible for this British StandardThe preparation of this British Standard was entrusted to Technical Committee TCI/80, Chemical testing of textiles, upon which the following bodies were represented:Association of Consulting ScientistsBritish Apparel and Textile C
5、onfederationBritish Measurement and Testing AssociationBritish Retail ConsortiumBS 6810-2:2005 BSI 31 October 2005ContentsPageCommittees responsible Inside front coverForeword ii1Scope 12 Normative references 13 Terms and definitions 14 General requirements 15 Extraction of soluble metals 26 Extract
6、ion of total metals 37 Determination of metals by atomic emission spectrophotometry 48 Test report 6Annex A (normative) Method of standard additions 7Bibliography 9Figure A.1 Example of calibration graph obtained using the method of standard additions 8Table 1 Wavelengths for atomic emission spectro
7、photometry 5iBS 6810-2:2005iiThis British Standard has been prepared by Technical Committee TCI/80.BS 6810 has been prepared in the context of several available test methods for the determination of metals in textiles by different analytical techniques. Part 1 of this standard covers the determinati
8、on of metals in textiles by the colorimetric and atomic absorption spectroscopy techniques. This Part of the standard describes the analysis of metals in textiles by atomic emission spectroscopy. It is applicable to a wide range of metals, being governed only by the wavelength range of the instrumen
9、t being used at low levels of concentration. A concentration range down to the sub parts per million level (mg/kg) in the sample can be realised for most metals. Methods of test for the determination of relatively large proportions of metals in textiles, such as may be introduced for proofing purpos
10、es, are covered by BS 2087-2, and BS 6F 100 also includes methods for the determination of traces of iron and copper.Chemical names in accordance with BS 2474 have been used, but deprecated names or other names used in industry are given, where applicable, in brackets.The presence of metallic elemen
11、ts in textile materials can arise in a variety of ways. Accidental or unforeseen contamination of textiles can occur, at any stage of manufacture or in use, by metals whose presence may pose a health hazard to humans or animals, particularly if the contamination is of such a nature that the metal is
12、 easily released. Some man-made fibres contain metals introduced in polymer manufacture (e.g. catalyst residues) or mass colouration (pigments). Animal fibres contain traces of copper, probably of biosynthetic origin. Metals can be deliberately introduced in subsequent processing (e.g. mordanting) o
13、r as components of metal-complex dyes. During textile processing, accidental contamination by materials of construction, notably copper and iron, is not uncommon, and can have a deleterious effect on quality. Methods of test for metals in textiles might be required for a variety of reasons related t
14、o the origins detailed above, quality control, fault diagnosis or complaint investigation, textile research and development work, or hygienic considerations.The methods for the determination of metals described in this standard are restricted to those that can be carried out in a well-equipped texti
15、le laboratory. Determination of metals in textile fibres, e.g. for general research purposes, for forensic investigations, and for the identification, through the presence of traces of metals deliberately introduced, of specific brands of man-made fibres, might not be covered by this standard.Assess
16、ed capability. Users of this standard are advised to consider the desirability of quality system assessment and registration against a recognized quality scheme such as BS EN ISO/IEC 17025 by an accredited third-party certification body.Warning This British Standard calls for the use of substances a
17、nd/or procedures that may be injurious to health if adequate precautions are not taken. It refers only to technical suitability and does not absolve the user from legal obligations relating to health and safety at any stage. Particular sources of hazard that require attention include the use of comp
18、ressed gases, the use of corrosive liquids at elevated temperatures, the handling of toxic substances, and the possibilities of explosive detonations in gases.It has been assumed in the drafting of this British Standard that the execution of its provisions is entrusted to appropriately qualified and
19、 experienced people.NOTE Good practice in relation to safety procedures is defined in Hazards in the chemical laboratory 1. Practical guidance in the application of COSHH regulations and broader aspects of health and safety in chemical laboratories are given in COSHH in laboratories 2 and Safe pract
20、ices in chemical laboratories 3. Foreword BSI 31 October 2005BS 6810-2:2005 BSI 31 October 2005A British Standard does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application.Compliance with a British Standard does not of itself confer imm
21、unity from legal obligations.Summary of pagesThis document comprises a front cover, an inside front cover, pages i to iii, a blank page, pages 1 to 9 and a back cover.The BSI copyright notice displayed in this document indicates when the document was last issued.iiiblankBS 6810-2:20051 ScopeThis Bri
22、tish Standard describes methods for the determination of the proportions present in commonly encountered textile fibres (excluding inorganic fibres) of metals, including the following metals: antimony, arsenic, barium, cadmium, chromium, cobalt, copper, iron, lead, manganese, mercury, nickel and zin
23、c. Methods are given for both soluble and total metals and are applicable to any metal capable of being detected by the instrumentation used.For atomic emission spectroscopy, the detection limit is governed by the calibration range chosen and the resolution of the instrumentation used.2 Normative re
24、ferencesThe following referenced documents are indispensable for the application of this document. For dated references, only the reference cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.BS 1752, Specification for laboratory si
25、ntered or fritted filters including porosity grading.BS 1792, Specification for one-mark volumetric flasks.BS 2586, Specification for glass and reference electrodes for the measurement of pH.BS 3145, Specification for laboratory pH meters.BS 4815, Glossary of generic names for man-made fibres.BS 681
26、0-1, Determination of metals in textiles Part 1: Analysis by atomic absorption and colorimetric spectroscopy.BS 6648, Methods for wet ashing of textile materials for subsequent determination of metal content.BS EN ISO 3696, Water for analytical laboratory use Specification and test methods.3 Terms a
27、nd definitionsFor the purposes of this British Standard, the terms and definitions given in BS 4815 apply, together with the following.3.1 total metal contentabsolute content of a metal in a fibre found by the dissolution of the fibre under specified conditions3.2 soluble metal contentcontent of a m
28、etal (excluding chromium) in the fibre that is soluble under specified conditions in hydrochloric acid, c(HCl) = 0.07 mol/l4 General requirements4.1 Choice and restrictions on the use of a method4.1.1 Preliminary treatment (see Clauses 5 and 6). If barium is sought, wet ashing (see 6.1) employing su
29、lfuric acid is not suitable, and dry ashing (see 6.2) shall be used. If barium is suspected to be present, dry ashing shall be used for the determination of other metals, except when mercury is the metal sought, when wet ashing shall be used.NOTE For the destruction of the organic material of textil
30、e fibres prior to the determination of metals, wet ashing is in general to be preferred, particularly when low levels of metals are being sought. Dry ashing, when its use is appropriate, has the advantage that it minimizes operator attention and avoids the use of large quantities of reagents and the
31、 high blank values that can result from their use.4.1.2 Determination of metals in the extract (see Clause 7). For the determination of mercury at low levels BSI 31 October 20051(0.5 ppm), atomic emission spectroscopy is not the recommended technique due to low sensitivity to this metal. Other techn
32、iques such as hydride generation are more applicable.NOTE For chromium, the soluble portion of the metal, which will be mostly in the hexavalent state, cannot be determined by atomic emission spectroscopy and should be determined colorimetrically (see Part 1 of this standard).BS 6810-2:20054.2 Equip
33、ment and reagentsUnless otherwise stated, reagents of recognized analytical quality shall be used and water conforming to a minimum of grade 2 of BS EN ISO 3696 shall be used. All purchased standard solutions shall be supplied with certificates of conformity; all solutions shall be prepared and stor
34、ed in accordance with Good Laboratory Practice.The apparatus shall be sound and clean. Glassware shall be made of chemically resistant glass. Caution Special attention needs to be paid to ensure cleanliness and the avoidance of contamination when carrying out the procedures described in this standar
35、d.NOTE For the determinations described in this standard, conditioning of samples before testing will not normally be necessary. If conditioning is agreed between the interested parties, it is recommended that the conditioning atmospheres defined in BS EN ISO 139 be used.5 Extraction of soluble meta
36、ls5.1 PrincipleFor all metals except chromium, the soluble metal content in the sample is extracted under defined conditions with hydrochloric acid, c(HCl) = 0.07 mol/l. Any buffering capacity that the sample might possess is compensated for by the addition of hydrochloric acid, c(HCl) approximately
37、 2 mol/l, so that the pH of the extract does not exceed 1.5.NOTE For the extraction of soluble metals, the ratios of mass of textile material to volume of extracting solution specified in 8.1.3 of BS EN 1413:1998 have been adopted.5.2 Reagents5.2.1 Hydrochloric acid, c(HCl) = 0.07 mol/l.5.2.2 Hydroc
38、hloric acid, c(HCl) approximately 2 mol/l. Dilute hydrochloric acid (approximately 37 % (m/m), density 1.18 g/ml), 166 ml in one litre water.5.2.3 Buffer solution, for standardization of the pH meter before measurement.NOTE These reagents are commercially available.5.3 Apparatus5.3.1 Conical flasks,
39、 capacity 100 ml or 250 ml, with ground glass joints and stoppers, as required.5.3.2 pH meter, conforming to BS 3145, used in conjunction with glass and reference electrodes conforming to BS 2586.5.3.3 Mechanical shaker, to agitate the mixture to ensure wetting out of the textile.5.3.4 Balance, accu
40、rate to 0.000 1 g.5.3.5 Source of heat, controllable at (40 2) C, e.g. a water bath.5.3.6 Coarse laboratory sintered filter, grade P250 conforming to BS 1752.5.3.7 One-mark volumetric flasks, capacities 100 ml and 250 ml, conforming to BS 1792.5.4 Procedure5.4.1 GeneralIf the amount of sample availa
41、ble permits, carry out the extraction in duplicate.2 BSI 31 October 2005BS 6810-2:20055.4.2 Soluble metals except chromiumCut the sample into pieces of such a size that all parts are readily wetted out. Weigh accurately a specimen of (2.5 0.05) g, and transfer it to a glass stoppered conical flask (
42、5.3.1).For wool in any textile form and felts and loose fibres, use a 250 ml flask and add (125 0.5) ml of hydrochloric acid (5.2.1) to the flask.For all other materials, use a 100 ml flask and add (50 0.2) ml of hydrochloric acid (5.2.1) to the flask.Agitate the flask by hand for a short period to
43、ensure that the textile is properly wetted out. For samples containing wool or polyamide, ensure that the pH of the extracting solution does not rise above 1.5; do this by measuring the approximate pH of the solution after the preliminary wetting out and carefully adding hydrochloric acid solution (
44、5.2.2) until the pH is 1.5 or less.NOTE If sufficient material is available, it might be more convenient to determine the quantity of additional acid required in a separate experiment.Shake the flask with the mechanical shaker (5.3.3) for one hour. Filter the extract through the coarse laboratory si
45、ntered filter (5.3.6). Rinse the filter and combine the rinsings and the extract.5.4.3 Preparation of the extract for analysisMake up the extract with a suitable volumetric flask with the solution used to prepare the extract.6 Extraction of total metals6.1 Wet ashing6.1.1 PrincipleThe procedure invo
46、lves the destruction of organic matter in the sample by controlled heating with a mixture of acids for the determination of the total metal content.6.1.2 ProcedureCarry out wet ashing in accordance with BS 6648. Do not subject the material to a preliminary charring procedure with sulfuric acid alone
47、 if arsenic is to be determined.Prepare a blank digest using the same quantities of reagents.6.2 Dry ashing6.2.1 PrincipleAn amount of the material, of known mass, is incinerated in a muffle furnace at a temperature not exceeding 450 C.6.2.2 Apparatus6.2.2.1 Silica, porcelain or platinum dish or cru
48、cible of suitable size.6.2.2.2 Temperature-controlled muffle furnace.6.2.2.3 Balance, accurate to 0.000 1 g. BSI 31 October 20053BS 6810-2:20056.2.3 ProcedurePlace a suitable weighed quantity of the material in the dish or crucible (6.2.2.1). Burn the material cautiously at the front of the open muf
49、fle furnace (6.2.2.2), taking care to avoid draughts, and when the material has reached the glowing stage move the dish towards the rear of the furnace, close the door, and complete the ashing at a temperature not exceeding 450 C (see Note 2).Warning Because of the possible evolution of toxic fumes in the slow ignition of some fibres, suitable ventilation shall be provided.NOTE 1 The mass of material used for the test is governed by the proportion present of the metal sought and the sensitivity of the method used fo
