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BS EN 17813:2023

$142.49

Environmental solid matrices. Determination of halogens and sulfur by oxidative pyrohydrolytic combustion followed by ion chromatography

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BSI 2023 24
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This document specifies an empirical method for the simultaneous direct determination of the fluorine, chlorine, bromine, and sulfur content in environmental solid matrices by oxidative pyrohydrolytic combustion at (1 050 Ā± 50) Ā°C, followed by ion chromatography. The method is applicable for the determination of concentrations ā‰„ 10 mg/kg of each element based on dry matter. The upper limit and exact concentration range covered depends on the blank levels of the instrumentation and the capacity of the chromatographic separation column used for determination. NOTE 1 Simultaneous determination of iodine content is possible but currently not validated. NOTE 2 Other detection methods can be applied if validated.

PDF Catalog

PDF Pages PDF Title
2 undefined
6 1 Scope
2 Normative references
3 Terms and definitions
4 Principle
7 5 Interferences
5.1 Interferences during combustion
5.2 Interferences during absorption
5.3 Interferences during ion chromatography
6 Reagents and gases
6.1 General
6.2 Reagents for ion chromatography
6.2.1 Eluents
8 6.2.2 Water, with a resistivity of ā‰„ 18 MĪ© cm (25 Ā°C)
6.2.3 Sodium carbonate (anhydrous), Na2CO3
6.2.3.1 Sodium carbonate concentrate, c(Na2CO3) = 0,09 mol/l
6.2.3.2 Sodium carbonate eluent, c(Na2CO3) = 0,009 mol/l
6.2.4 Bromide, chloride, fluoride, and sulfate stock solutions, c = 1 000 mg/l of each anion
6.2.5 Bromide, chloride, fluoride, and sulfate standard solutions
6.2.5.1 General
6.2.5.2 Example of a bromide, chloride, fluoride, and sulfate mixed standard solution, c = 100 mg/l of each anion
9 6.2.5.3 Example of bromide, chloride, fluoride, and sulfate mixed calibration solutions
6.3 Reagents and gases for combustion
6.3.1 Inert gas, for example argon, ā‰„ 99,9 % (v/v) purity
6.3.2 Oxygen, ā‰„ 99,9 % (v/v) purity
6.4 Control standard
6.4.1 General
6.4.2 4-Bromobenzoic acid, C7H5BrO2, ā‰„ 99 % (m/m) purity, CAS no. 586-76-5
6.4.3 4-Chlorobenzoic acid, C7H5ClO2, ā‰„ 99 % (m/m) purity, CAS no. 74-11-3
6.4.4 Dibenzothiophene, C12H8S, ā‰„ 99 % (m/m) purity, CAS no. 132-65-0
6.4.5 4-Fluorobenzoic acid, C7H5FO2, ā‰„ 99 % (m/m) purity, CAS no. 456-22-4
6.4.6 Xylene, C8H10, analytical grade, CAS no. 1330-20-7
6.4.7 Example of a bromine, chlorine, fluorine, and sulfur control standard solution, c = 1 000 mg/l of each element
6.4.8 Example of a bromine, chlorine, fluorine, and sulfur control standard solution, c = 10 mg/l and 100 mg/l of each element
10 6.5 Reagents for absorption
6.5.1 General
6.5.2 Hydrogen peroxide solution, H2O2, approx. 30 % (m/m), electronic grade
6.5.2.1 Absorption solution containing hydrogen peroxide, c(H2O2) ā‰ˆ 330 mg/l
6.5.3 Sodium methane sulfonate, CH3SO3Na
6.5.3.1 Sodium methane sulfonate solution, c(CH3SO3Na) = 500 mg/l
6.5.3.2 Absorption solution containing sodium methane sulfonate, c(CH3SO3Na) = 1 mg/l
7 Apparatus
7.1 Combustion apparatus
7.1.1 Combustion furnace
11 7.1.2 Combustion vessel
7.1.3 Absorption vessel
7.2 Ion chromatography (IC) system
7.2.1 General
12 7.2.2 Eluent storage container
7.2.3 High pressure pump
7.2.4 Sample injection system
7.2.5 Guard column
7.2.6 Separation column
7.2.7 Conductivity detector and suppressor device
7.2.8 Data handling unit
7.2.9 Quality of the separation system
13 8 Sampling and sample preparation
9 Procedure
9.1 Combustion
9.1.1 General
14 9.1.2 Blank determination
9.2 Absorption
9.3 Ion chromatography
9.3.1 General
9.3.2 Calibration
15 9.3.3 Measurement
9.4 Initial and daily checks
9.4.1 Initial laboratory capability check
9.4.2 Daily check
16 10 Calculation
11 Expression of result
12 Test report
17 Annex A (informative)Performance characteristics
BS EN 17813:2023
$142.49