ASTM E1787-2008 Standard Test Method for Anions in Caustic Soda and Caustic Potash (Sodium Hydroxide and Potassium Hydroxide) by Ion Chromatography《离子色谱法测定苛性钠和苛性碱(氢氧化钠和氢氧化钾)中阴离子的标准.pdf
《ASTM E1787-2008 Standard Test Method for Anions in Caustic Soda and Caustic Potash (Sodium Hydroxide and Potassium Hydroxide) by Ion Chromatography《离子色谱法测定苛性钠和苛性碱(氢氧化钠和氢氧化钾)中阴离子的标准.pdf》由会员分享,可在线阅读,更多相关《ASTM E1787-2008 Standard Test Method for Anions in Caustic Soda and Caustic Potash (Sodium Hydroxide and Potassium Hydroxide) by Ion Chromatography《离子色谱法测定苛性钠和苛性碱(氢氧化钠和氢氧化钾)中阴离子的标准.pdf(6页珍藏版)》请在麦多课文档分享上搜索。
1、Designation: E 1787 08Standard Test Method forAnions in Caustic Soda and Caustic Potash (SodiumHydroxide and Potassium Hydroxide) by IonChromatography1This standard is issued under the fixed designation E 1787; the number immediately following the designation indicates the year oforiginal adoption o
2、r, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This test method covers the determination of anionicimpurities in 50 % causti
3、c soda (sodium hydroxide) and 50 %caustic potash (potassium hydroxide) solutions using ionchromatography (IC). Anions that can be determined at con-centrations of approximately 0.11000 ug/g (ppm) include:bromide, chlorate, chloride, fluoride, nitrate, phosphate, andsulfate.1.2 By varying the sample
4、size, this test method can be usedfor anhydrous caustic soda and caustic potash products, as wellas other concentrations of liquid products.1.3 This test method is not intended to be used to quantifychloride in caustic soda where the sodium chloride concentra-tion is approximately 1 %. For the most
5、accurate determina-tions, it is recommended that high concentrations of chloridebe analyzed using a potentiometric titration procedure, such asthe one described in Test Methods E 291.1.4 The values stated in SI units are to be regarded asstandard. The values given in parentheses are for informationo
6、nly.1.5 Review the current appropriate Material Safety DataSheets (MSDS) for detailed information concerning toxicity,first aid procedures, and safety precautions.1.6 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the
7、user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Specific hazardsstatements are given in Section 8.2. Referenced Documents2.1 ASTM Standards:2D 1193 Specification for Reagent WaterE 180 Practice for D
8、etermining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty ChemicalsE 291 Test Methods for Chemical Analysis of Caustic Sodaand Caustic Potash (Sodium Hydroxide and PotassiumHydroxide)3. Summary of Test Method3.1 Bromide, chlorate, chloride, fluoride, nitrate, phos
9、phateand sulfate are measured in NaOH or KOH by ion chromatog-raphy. The sample solution is diluted and injected onto asample loop of an automated neutralization module. Thesample in the loop is pumped to a suppression device whichuses electrolysis to neutralize the hydroxide ions. The samplethen is
10、 circulated through this device several times until it iscompletely neutralized. Anionic constituents of the neutralizedsample are concentrated on an anion concentrator column.After the concentration they are separated into individualelution bands in the eluent on a separator column. Theconductivity
11、 of the eluent is reduced with an anion suppressiondevice, and the anions of interest are detected using a conduc-tivity detector. Quantitation of the anions in the samplesolution is achieved by calibrating the IC with a series ofstandards containing known amounts of the anions. Thesestandards are a
12、lso passed through the neutralization device.4. Significance and Use4.1 Anion impurities in caustic soda and caustic potash aremonitored by manufacturers and users for quality control of theproducts.Anions of primary interest are chloride, chlorate, andsulfate. This test method has determined precis
13、ion estimatesonly for these three impurities.5. Interferences5.1 Substances that coelute with the anions of interest willinterfere. A high concentration of one anion can interfere withaccurate quantitation of another anion if their retention timesare close and resolution is affected. For example, ca
14、ustic sodasamples containing large concentrations of chloride can inter-fere with the quantitation of small amounts of fluoride.Selection of a high capacity anion separator column willminimize this problem.1This test method is under the jurisdiction of ASTM Committee E15 onIndustrial and Specialty C
15、hemicals and is the direct responsibility of SubcommitteeE15.01 on General Standards.Current edition approved April 1, 2008. Published May 2008. Originallypublished in 1996. Last previous edition approved in 2002 as E 1787-02.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orco
16、ntact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, We
17、st Conshohocken, PA 19428-2959, United States.5.2 Organic acids, surfactants, dyes, metals, etc., can causefouling of the columns and membranes used in this testmethod, resulting in interferences and decreased sensitivity. Itis very important to follow the manufacturers recommenda-tions for cleaning
18、 and maintaining the various parts of the ICsystem.5.3 The anion concentrator column in the neutralizationmodule has a finite capacity for trapping anions, approximately25 micro-equivalents per column. When the capacity of thecolumn is exceeded, the stripping of anions will not bequantitative.6. App
19、aratus6.1 Ion Chromatograph, equipped with:6.1.1 Conductivity Detector,6.1.2 Anion Separator Column,6.1.3 Guard Column,6.1.4 100-L Sample Loop,6.1.5 Autoneutralization Device, capable of neutralizing thecaustic sample prior to being directed through the separatorcolumn,6.1.6 Post-Column Chemical Sup
20、pression Device, capableof reducing background conductivity due to the eluent, and6.1.7 Data Acquisition System, such as an integrator orcomputer system.6.2 100-mL Volumetric Flasks, for preparing sample solu-tions.6.3 Disposable 10-mL Syringes, for injecting solution intothe IC.6.3.1 IC Autosampler
21、 (optional), can be used as an alterna-tive to manually injecting samples.7. Reagents7.1 Purity of ReagentsReagent grade chemicals should beused in all tests. Unless otherwise indicated, all reagents mustconform to the specifications of the Committee on AnalyticalReagents of the American Chemical So
22、ciety, where suchspecifications are available.3Other grades may be used pro-vided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.7.2 Purity of WaterReferences to water means Type 1 (18MV-cm deionized water)
23、conforming to Specification D 1193.7.3 Anion Stock Standards, 1000 ug/g (ppm):7.3.1 Bromide Stock Solution (1.00 mL = 1.00 mgBromide)Dry sodium bromide (NaBr) for 6 h at 150C andcool in a desiccator. Dissolve 1.288 g of the dried NaBr inwater, dilute to 1 L with water, and mix well.7.3.2 Chlorate St
24、ock Solution (1.00 mL = 1.00 mgChlorate)Dissolve 1.275 g of sodium chlorate (NaClO3)inwater, dilute to 1 L with water, and mix well.7.3.3 Chloride Stock Solution (1.00 mL = 1.00 mgChloride)Dry sodium chloride (NaCl) for1hat100C andcool in a desiccator. Dissolve 1.648 g of the dried NaCl inwater, dil
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