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Standard Test Method for Anions in Water by Suppressed Ion Chromatography 用抑制离子色谱法测定水中阴离子的标准试验方法
发布日期: 2017-12-01
1.1 本试验方法 2. , 3. 包括氟化物、氯化物、亚硝酸盐、, 正交 -抑制离子色谱法测定水中的磷酸盐、溴化物、硝酸盐和硫酸盐离子。 注1: 洗脱顺序取决于使用的色谱柱;看见 图1 . 1.3 用户有责任确保该测试方法对其他矩阵的有效性。 1.4 根据待量化的阴离子,在单个实验室工作中测定低至0.01 mg/L的浓度。利用50μL样品体积回路和3000μS/cm满标度的灵敏度,近似检测限如所示 表1 可以实现。较新的仪器、色谱柱技术和洗脱液的检测限较低。分析员必须确保最佳仪器性能,以在更灵敏的电导率下保持稳定的基线- 比例设置。 (A) 数据由俄亥俄州辛辛那提的美国环境保护局/EMSL实验室提供。 (B) 列:如中所述 7.1.4 . 探测器:如 7.1.6 . 洗脱液:如 8.3 . 泵速:2.0毫升/分钟。 样品回路:50μL。 1.5 本试验方法的上限取决于总阴离子浓度,并可按中所述通过实验确定 附件A1 . 可通过适当稀释或使用较小的注射量来延长这些限制。 1.6 使用交替的分离柱和洗脱液可以测定其他阴离子,如醋酸盐、甲酸盐或柠檬酸盐。这不是本试验方法的主题。 1.7 本试验方法更新批准使用电解生成的洗脱液、电解再生的洗脱液、电解抑制(非自动调零)和电解捕集柱(也称为试剂)- 自由离子色谱法。本批准基于美国环境保护局的验收,参考 附录X2 . 1.8 以国际单位制表示的数值应视为标准值。本标准不包括其他计量单位。 1.9 本标准并非旨在解决与其使用相关的所有安全问题(如有)。本标准的用户有责任在使用前制定适当的安全、健康和环境实践,并确定监管限制的适用性。 1.10 本国际标准是根据世界贸易组织技术性贸易壁垒(TBT)委员会发布的《关于制定国际标准、指南和建议的原则的决定》中确立的国际公认标准化原则制定的。 ====意义和用途====== 5.1 离子色谱法可对七种常见阴离子F进行定性和定量测定 − ,Cl − ,否 2. − ,HPO 4. −2. ,Br − ,否 3. − ,等等 4. −2. ,在毫克/升范围内,从只需要几毫升样品的单个分析操作开始,大约需要10到15分钟才能完成。还可以量化附加阴离子,例如羧酸。 注2: 如果氟化物的峰值在水浸液中,则可使用本试验方法测定氟化物,方法是添加1 mL洗提液(浓度为100×10-1) 8.3 )所有100毫升体积的样品和标准品,以消除浸水的影响。(参见 6.3 ,另请参见 6.4 .) 应避免对未恢复的峰进行定量。 阴离子,如低分子量有机酸(甲酸盐、醋酸盐、丙酸盐等),与氟化物共价导电,会影响某些饮用水和大多数废水中氟化物的定量。如果采取措施去除使用碳酸盐基洗脱液抑制后残留在洗脱液中的碳酸,则可以进一步减少水浸。如果使用氢氧化物洗脱液,则不需要水浸。 5.2 阴离子组合,如Cl − /Br − 而且没有 2. − /没有 3. − 离子色谱法可以很容易地将其他分析方法难以区分的杂质分离出来。
1.1 This test method 2 , 3 covers the sequential determination of fluoride, chloride, nitrite, ortho -phosphate, bromide, nitrate, and sulfate ions in water by suppressed ion chromatography. Note 1: Order of elution is dependent upon the column used; see Fig. 1 . 1.3 It is the user's responsibility to ensure the validity of this test method for other matrices. 1.4 Concentrations as low as 0.01 mg/L were determined depending upon the anions to be quantified, in single laboratory work. Utilizing a 50-μL sample volume loop and a sensitivity of 3000 μS/cm full scale, the approximate detection limits shown in Table 1 can be achieved. Lower detection limits have been observed with newer instrumentation, column technology and eluents. The analyst must assure optimum instrument performance to maintain a stable baseline at more sensitive conductivity full-scale settings. (A) Data provided by U.S. EPA/EMSL Laboratory, Cincinnati, OH. (B) Column: as specified in 7.1.4 . Detector: as specified in 7.1.6 . Eluent: as specified in 8.3 . Pump rate: 2.0 mL/min. Sample loop: 50 μL. 1.5 The upper limit of this test method is dependent upon total anion concentration and may be determined experimentally as described in Annex A1 . These limits may be extended by appropriate dilution or by use of a smaller injection volume. 1.6 Using alternate separator column and eluents may permit additional anions such as acetate, formate, or citrate to be determined. This is not the subject of this test method. 1.7 This test method update approves the use of electrolytically generated eluent, electrolytically regenerated eluent, electrolytic suppression (not autozeroing), and electrolytic trap columns also known as reagent-free ion chromatography. This approval is based on acceptance by the U.S. EPA as referenced in Appendix X2 . 1.8 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. 1.9 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. 1.10 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee. ====== Significance And Use ====== 5.1 Ion chromatography provides for both qualitative and quantitative determination of seven common anions, F − , Cl − , NO 2 − , HPO 4 −2 , Br − , NO 3 − , and SO 4 −2 , in the milligram per litre range from a single analytical operation requiring only a few millilitres of sample and taking approximately 10 to 15 min for completion. Additional anions, such as carboxylic acids, can also be quantified. Note 2: This test method may be used to determine fluoride if its peak is in the water dip by adding 1 mL of eluent (at 100× the concentration in 8.3 ) to all 100-mL volumes of samples and standards to negate the effect of the water dip. (See 6.3 , and also see 6.4 .) The quantitation of unretained peaks should be avoided. Anions such as low molecular weight organic acids (formate, acetate, propionate, etc.) that are conductive coelute with fluoride and would bias fluoride quantitation in some drinking waters and most wastewaters. The water dip can be further minimized if measures are taken to remove carbonic acid which remain in the eluent after suppression using carbonate based eluents. There is no water dip if hydroxide eluents are used. 5.2 Anion combinations such as Cl − /Br − and NO 2 − /NO 3 − , which may be difficult to distinguish by other analytical methods, are readily separated by ion chromatography.
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归口单位: D19.05
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