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Standard Test Methods for Trace Anions in High Purity Water by Ion Chromatography 通过离子色谱法测定高纯度水中痕量阴离子的标准测试方法
发布日期: 2016-06-01
1.1 这些测试方法包括使用离子色谱法结合样品预浓缩测定高纯度水中痕量(μg/L)的氟化物、醋酸盐、甲酸盐、氯化物、磷酸盐和硫酸盐。其他阴离子,如溴化物、亚硝酸盐、硝酸盐、亚硫酸盐和碘化物,可通过该方法测定。然而,由于它们在高纯度水中很少以显著浓度存在,因此不包括在本试验方法中。本文介绍了两种测试方法,其应用范围由协作研究确定,如下所示: 测试范围 (添加μg/L) 检测极限 A. (单个操作员) (微克/升) 小节 试验方法A: 7. – 16 氯化物 0–24 0.8 磷酸盐 0–39 B 硫酸盐 0–55 1.8 试验方法B: 17 – 24 氟化物 0–14 0.7 醋酸盐 0–414 6.8 甲酸盐 0–346 5.6 (A) 检测限为最低可测量浓度,99时不报告为零 % 第节引用的EPRI研究的置信度 16 和 24 . (B) 数据不足,无法计算检测极限。 1.2 用户有责任确保这些测试方法对未经测试的基质水的有效性。 1.3 试验方法A的常见实用范围如下:氯化物,1至100μg/L,磷酸盐,3至100μg/L,硫酸盐,2至100μg/L。 1.4 试验方法B的常见实用范围如下:氟化物,1至100μg/L,醋酸盐,10至200μg/L,甲酸盐,5至200μg/L。 1.5 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。 1.6 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和健康实践,并确定监管限制的适用性。 ====意义和用途====== 4.1 阴离子氟化物、氯化物和硫酸盐已被确定为导致高压锅炉、电力涡轮机及其相关热交换器腐蚀的重要因素。 许多电力公司试图将锅炉给水中的这些污染物减少到1μg/L以下。 4.2 在半导体制造过程中,除其他外,这些离子已被确定为产品产量低的原因,因此,必须对其进行监测和控制,使其达到与电力行业所要求的水平相似的水平。 4.3 在许多蒸汽发生器给水和冷凝液中发现了低分子量有机酸,如醋酸盐和甲酸盐。据信,它们来自锅炉补给水中发现的有机物的高温分解。人们认为,这些有机酸通过降低锅炉水的pH值来促进腐蚀,甚至可能本身具有腐蚀性。 4.4 当紫外线用于生产用于半导体加工的无菌水时,也可能产生这种低分子量有机物。这种极性有机污染物被怀疑会导致半导体产量下降。 4.5 磷酸盐通常以低mg/L的水平添加到汽包锅炉中,以沉淀钙和镁,从而防止结垢。离子色谱法可用于监测锅炉水中此类化学品的浓度,以及检测进入蒸汽中的有害残留物。
1.1 These test methods cover the determination of trace (μg/L) levels of fluoride, acetate, formate, chloride, phosphate, and sulfate in high purity water using ion chromatography in combination with sample preconcentration. Other anions, such as bromide, nitrite, nitrate, sulfite, and iodide can be determined by this method. However, since they are rarely present in significant concentrations in high purity water, they are not included in this test method. Two test methods are presented and their ranges of application, as determined by a collaborative study, are as follows: Range Tested (μg/L Added) Limit of Detection A (Single Operator) (μg/L) Sections Test Method A: 7 – 16 Chloride 0–24 0.8 Phosphate 0–39 B Sulfate 0–55 1.8 Test Method B: 17 – 24 Fluoride 0–14 0.7 Acetate 0–414 6.8 Formate 0–346 5.6 (A) Limit of detection is lowest measurable concentration not reportable as zero at 99 % level of confidence as per EPRI study as cited in Sections 16 and 24 . (B) Insufficient data to calculate limit of detection. 1.2 It is the user's responsibility to ensure the validity of these test methods for waters of untested matrices. 1.3 The common practical range of Test Method A is as follows: chloride, 1 to 100 μg/L, phosphate, 3 to 100 μg/L, and sulfate, 2 to 100 μg/L. 1.4 The common practical range of Test Method B is as follows: fluoride, 1 to 100 μg/L, acetate, 10 to 200 μg/L, and formate, 5 to 200 μg/L. 1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. 1.6 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 and health practices and determine the applicability of regulatory limitations prior to use. ====== Significance And Use ====== 4.1 The anions fluoride, chloride, and sulfate have been identified as important contributors to corrosion of high pressure boilers, electric power turbines and their associated heat exchangers. Many electric power utilities attempt to reduce these contaminants in their boiler feed water to less than 1 μg/L. 4.2 In the semiconductor manufacturing process these ions, among others, have been identified as a cause of low product yield and, thus, must be monitored and controlled to levels similar to those required by the electric power industry. 4.3 Low molecular weight organic acids, such as acetate and formate, have been found in many steam generator feed waters and condensates. They are believed to come from the high temperature breakdown of organic matter found in boiler make up water. It is felt that these organic acids promote corrosion by lowering the pH of boiler waters and may even be corrosive themselves. 4.4 Such low molecular weight organics may also be produced when ultraviolet light is used to produce bacteria-free water for semiconductor processing. Such polar organic contaminants are suspected of causing reduced semiconductor yields. 4.5 Phosphates are commonly added to drum boilers in the low mg/L level to precipitate calcium and magnesium and thereby prevent scale formation. Ion chromatography can be used to monitor the concentration of such chemicals in boiler water, as well as detect unwanted carry-over into the steam.
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归口单位: D19.03
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