SANS 5209-2010 Water - Manganese content《水 锰含量》.pdf

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3、damage whatsoever than may result from the use of this material or the information contain therein, irrespective of the cause and quantum thereof. ISBN 978-0-626-24305-0 SANS 5209:2010Edition 3.2SOUTH AFRICAN NATIONAL STANDARD Water Manganese content Published by SABS Standards Division 1 Dr Lategan

4、 Road Groenkloof Private Bag X191 Pretoria 0001Tel: +27 12 428 7911 Fax: +27 12 344 1568 www.sabs.co.za SABS SANS 5209:2010 Edition 3.2 Table of changes Change No. Date Scope Amdt 1 2005 Amended to change the designation of SABS standards to SANS standards and to update referenced standards. Amdt 2

5、2010 Amended to update referenced standards. Foreword This South African standard was approved by National Committee SABS SC 147A, Water Water sampling and analysis, in accordance with procedures of the SABS Standards Division, in compliance with annex 3 of the WTO/TBT agreement. This document was p

6、ublished in March 2010. This document supersedes SANS 5209:2005 (edition 3.1). A vertical line in the margin shows where the text has been technically modified by amendment No. 2. SANS 5209:2010 Edition 3.2 1 Water Manganese content 1 Scope and field of application This standard specifies a method o

7、f determining the manganese content of water and wastewater, using an air-acetylene flame and direct flame atomic absorption. The method is applicable to the determination of manganese in the concentration range 0,05 mg/L to 5,0 mg/L. 2 Normative references The following referenced documents are ind

8、ispensable 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. Information on currently valid national and international standards can be obtained from th

9、e SABS Standards Division. Amdt 1 SANS 111/ISO 835, Laboratory glassware Graduated pipettes. Amdt 1; amdt 2 SANS 112/ISO 648, Laboratory glassware Single volume pipettes. Amdt 1 SANS 115/ISO 385, Laboratory glassware Burettes. Amdt 1; amdt 2 SANS 128/ISO 1042, Laboratory glassware One-mark volumetri

10、c flasks. Amdt 1 SANS 3696/ISO 3696, Water for analytical laboratory use Specification and test methods. SANS 6168, Water Pretreatment for metal analysis. 3 Principle The pretreated sample is aspirated into an air-acetylene flame under oxidizing conditions and the absorbance measured at 279,5 nm is

11、compared with the absorbances of manganese standards measured under the same conditions. Interference by silica is inhibited by the addition of calcium to the sample. 4 Reagents NOTE Unless otherwise specified, only use water that complies with the requirements of SANS 3696 and reagents of analytica

12、l reagent grade. SANS 5209:2010 Edition 3.2 2 4.1 Nitric acid (HNO3) Concentrated (d at 25 /25 C = 1,42). 4.2 Hydrochloric acid (HCl) Concentrated (d at 25 /25 C = 1,19). 4.3 Dilute hydrochloric acid 1 + 4 HCl. 4.4 Acidified water Containing 1,5 mL of HNO3(see 4.1) per litre. 4.5 Calcium carbonate s

13、olution Dissolve 0,63 g of calcium carbonate (CaCO3) in 50 mL of the dilute HCl (see 4.3). If necessary, heat and boil gently to dissolve completely. Cool and dilute with water to 1 000 mL in a volumetric flask. 4.6 Manganese stock solution (1 000 mg/L) 4.6.1 Obtain a commercially available stock so

14、lution of manganese (1 000 mg/L) of guaranteed quality, or prepare the stock solution as described in 4.6.2. 4.6.2 Dissolve 3,076 g of manganous sulfate monohydrate (MnSO4H2O), previously dried in a desiccator for 24 h, in 200 mL of water. Add 1,5 mL of HNO3(see 4.1) and dilute with water to 1 000 m

15、L in a volumetric flask. 4.7 Manganese working stock solution (100 mg/L) Pipette 10,0 mL of the stock solution (see 4.6) into a 100 mL volumetric flask and dilute to the mark with the acidified water (see 4.4). 4.8 Manganese standard solutions (0,05 mg/L to 5,0 mg/L) 4.8.1 Prepare at least three man

16、ganese standard solutions that will bracket the expected concentration of the sample by dilution of the working stock solution (see 4.7), using the acidified water (see 4.4) as the diluent. 4.8.2 Add 25,0 mL of the CaCO3solution (see 4.5) per 100 mL of each standard. 5 Apparatus 5.1 Atomic absorptio

17、n spectrophotometer, for use at 279,5 nm. 5.2 Air-acetylene burner, suitable for attachment to the spectrophotometer (see 5.1). 5.3 Manganese hollow-cathode lamp. 5.4 Oxidant, air, dried and filtered. SANS 5209:2010 Edition 3.2 3 5.5 Fuel, acetylene, standard commercial grade. (Replace the cylinder

18、when the cylinder pressure drops to 700 kPa.) CAUTION: Never allow the operating pressure of acetylene to exceed 105 kPa. 5.6 Pressure-reducing regulators, for the supply of fuel and oxidant to the instrument at the appropriate levels recommended by the manufacturer. 5.7 Glassware. Where applicable,

19、 only use burettes, pipettes and volumetric flasks that comply with the requirements for class A items as specified in SANS 111, SANS 112, SANS 115 and SANS 128, as relevant. Amdt 1; amdt 2 6 Sample pretreatment 6.1 Pretreat the sample, a blank (see 4.4) and at least one standard (see 4.8.1) in acco

20、rdance with SANS 6168 in order to analyse for the appropriate form of metal, i.e. soluble, insoluble or total metal. NOTE For the purposes of legislation or specifications relating to this method, pretreat the sample for recovery of total manganese, unless specifically indicated otherwise. 6.2 Add 2

21、5,0 mL of the CaCO3solution (see 4.5) per 100 mL of each sample, standard(s) and blank after pretreatment as in 6.1, and mix well. 7 Procedure 7.1 Instrument operation NOTE The differences between makes and models of atomic absorption spectrophotometers make it impracticable to formulate detailed op

22、erating instructions. Follow the manufacturers operating instructions for the specific instrument but, in general, proceed in accordance with the instructions given in 7.1.1 to 7.1.10. 7.1.1 Turn on the instrument, install the manganese hollow-cathode lamp (see 5.3) and apply the current recommended

23、 by the manufacturer. 7.1.2 Set the wavelength at 279,5 nm and set the slit width in accordance with the manufacturers instructions. 7.1.3 Allow the lamp to stabilize for approximately 10 min and then align it to obtain optimum transmission. 7.1.4 Adjust the fine control of the wavelength setting of

24、 the monochromator in order to ensure maximum response. 7.1.5 Install the air-acetylene burner (see 5.2). 7.1.6 Check and, if necessary, adjust the gas flow rates to ensure that they are at the levels specified for the instrument. 7.1.7 Turn on the air supply and then the acetylene flow, and ignite

25、the mixture. 7.1.8 Ensure that the flame is oxidizing (non-luminous with a hazy blue inner core), and then zero the instrument in the absorbance mode. SANS 5209:2010 Edition 3.2 4 7.1.9 Aspirate a standard that will give an absorbance exceeding 0,2, and optimize the burner position until the maximum

26、 absorbance value is recorded. The instrument is now ready for calibration and analysis. 7.1.10 After analysis, extinguish the flame by turning off the acetylene flow first. When the flame is extinguished, turn off the air supply. 7.2 Instrument calibration 7.2.1 Aspirate the analyte blank (see 4.4)

27、 and zero the instrument. 7.2.2 Aspirate each of the standard solutions (see 4.8.2), using the acidified water (see 4.4) to flush the nebulizer between aspirations, and record their respective absorbances. 7.2.3 Construct a calibration curve, using the standard concentrations and their respective ab

28、sorbances. 7.3 Sample analysis 7.3.1 Aspirate the pretreated blank, standard(s) and sample (see 6.2), using the acidified water (see 4.4) to flush the nebulizer between aspirations. 7.3.2 Record the absorbances and determine the concentrations by referring to the calibration curve as constructed in

29、7.2.3, or record the concentrations directly if an instrument with concentration mode is used. 7.3.3 Correct the results for the sample and the control standard(s) by subtracting the result for the pretreated blank, if applicable, and verify the absence of interference due to the pretreatment method

30、 by confirmation of the true concentration(s) of the control standard(s). 8 Expression of results So express the result as to indicate the form of metal analysed and the concentration units used, e.g. Total manganese as Mn in mg/L. SABS SABS Standards Division The objective of the SABS Standards Div

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