1、Designation: D5544 11D5544 16Standard Test Method forOn-Line Measurement of Residue After Evaporation of High-Purity Water1This standard is issued under the fixed designation D5544; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, t
2、he 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. Scope1.1 This test method covers the determination of dissolved organic and inorganic matter and colloidal material
3、found inhigh-purity water used in the semiconductor, and related industries. This material is referred to as residue after evaporation (RAE).The range of the test method is from 0.001 g/L(ppb) g/L (ppb) to 60 g/L (ppb).1.2 This test method uses a continuous, real time monitoring technique to measure
4、 the concentration of RAE. A pressurizedsample of high-purity water is supplied to the test methods apparatus continuously through ultra-clean fittings and tubing.Contaminants from the atmosphere are therefore prevented from entering the sample. General information on the test method anda literature
5、 review on the continuous measurement of RAE has been published.21.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.mathematical conversions to inch-pound units that are provided for information only and are not considered s
6、tandard.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. For spec
7、ific hazards statements, see Section 8.2. Referenced Documents2.1 ASTM Standards:3D1129 Terminology Relating to WaterD2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on WaterD3370 Practices for Sampling Water from Closed ConduitsD3864 Guide for On-Li
8、ne Monitoring Systems for Water AnalysisD3919 Practice for Measuring Trace Elements in Water by Graphite Furnace Atomic Absorption SpectrophotometryD5127 Guide for Ultra-Pure Water Used in the Electronics and Semiconductor IndustriesE1184 Practice for Determination of Elements by Graphite Furnace At
9、omic Absorption Spectrometry3. Terminology3.1 DefinitionsFor definitions of terms used in this test method, refer to Terminology D1129.3.2 Definitions of Terms Specific to This Standard:3.2.1 aerosol, nany solid or liquid particles, with a nominal size range from 10 nm to 100 m, suspended in a gas (
10、usuallyair).3.2.2 colloidal suspension, nany material in suspension (for example, silica) with a nominal particle size less than 100 nm.3.2.3 Water-based condensation particle counter (WCPC), ninstrument for detecting very small aerosol particles in a sizerange from approximately 7 nm to 2 to 3 m.1
11、This test method is under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.03 on Sampling Water andWater-Formed Deposits, Analysis of Water for Power Generation and Process Use, On-Line Water Analysis, and Surveillance of Water.Current edition appr
12、oved May 1, 2011June 1, 2016. Published May 2011June 2016. Originally approved in 1994. Last previous edition approved in 20052011 asD5544 05.D5544 11. DOI: 10.1520/D5544-11.10.1520/D5544-16.2 Blackford, D. B., “Use of Nonvolatile Residue Monitoring in Semiconductor Water Applications” Ultrapure Wat
13、er Journal, November 2008 pp 16-23 Published by TallOaks PublishingBlackford, D. B., “Use of Nonvolatile Residue Monitoring in Semiconductor WaterApplications” Ultrapure Water Journal, Tall Oaks Publishing, November2008, pp. 1623.3 For referencedASTM standards, visit theASTM website, www.astm.org, o
14、r contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes ha
15、ve been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official do
16、cument.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.2.3.1 DiscussionThe WCPC cannot differentiate among particles of varying size within this size range; the counter reports the number of particleswith a size greater than that de
17、fined by the detection-efficiency curve. Detection is independent of particle composition.3.2.4 detection effciency, nin this test method, detection efficiency represents a curve relating particle size to a countersability to detect that size.3.2.5 polydisperse, adja type of size population, in this
18、 case of aerosol particles, composed of many different sizes; theopposite of monodisperse, which is a type of size distribution of just one size.3.2.6 realtime, nthe time that an event is occurring plus the response time.3.2.6.1 DiscussionIn this case, the response time is 3 to 5 min, therefore, con
19、tamination is recorded 3 to 5 min after it occurs.3.2.7 residue after evaporation, ncontaminants remaining after all water is evaporated; sometimes known as nonvolatileresidue or total dissolved and suspended solids.4. Summary of Test Method4.1 This test method consists of continuously removing a re
20、presentative sample of high-purity water from a pressurized supplyline (refer to Practices D3370, Practice C on Continual Sampling, and Practice D3864). The temperature of the incominghigh-purity water should ideally be at room temperature, but not more than 50C.Anebulizer is supplied with the high-
21、purity waterat a constant flow rate, and a source of compressed air, or nitrogen, at a constant flow rate and pressure, to generate a stable aerosolof high-purity water droplets. Under these conditions, the nebulizer produces a polydisperse size distribution of droplets with amedian size of approxim
22、ately 1 m, and a concentration of approximately 107 droplets/s, or 1012 droplets/mL4.2 The droplets are heated at 120C. . After the heating, additional compressed air or nitrogen is introduced from the supplyto prevent re-condensation and to quickly move the residue particles to the Water-based Cond
23、ensation Particle Counter (WCPC).4.3 The WCPC works as follows: Residue particles pass through a region called the Saturator (see Fig. 1) where the residueparticles are saturated with water vapor and temperature equilibrated. The residue particles and water vapor then pass into a regioncalled the Gr
24、owth Tube, where the wetted walls of the porous media are heated to raise vapor pressure. The high diffusivity of thevapor allows it to reach the center of the sample stream at a faster rate than the thermal diffusivity of the vapor can equilibrateto the higher temperatures near the walls, resulting
25、 in a supersaturated condition along the radius of the flow stream. Residueparticles in the flow stream act as nuclei for condensation. Water condenses on the residue particles to form large droplets withonly one residue particle at the center of each droplet. Droplets can then be counted with a rel
26、atively simple optical particle counter.A more elaborate description of the WCPCs method for distinguishing between clean and dirty water is described in AppendixX1.4.4 A calibration technique (described in detail in Section 10) uses concentration standards of high-purity potassium chloride(KCl) to
27、convert the WCPC count concentration in particles per cubic centimetre into RAE concentration in micrograms per litreor milligrams per litre. A graphite furnace atomic absorption spectrometer (GFAAS), or equivalent method, can be used to checkthe concentration of KCl in this test method standard (se
28、e Practices D3919 and E1184).5. Significance and Use5.1 Even so-called high-purity water will contain contaminants. While not always present, these contaminants may contributeone or more of the following: dissolved active ionic substances such as calcium, magnesium, sodium, potassium, manganese,ammo
29、nium, bicarbonates, sulfates, nitrates, chloride and fluoride ions, ferric and ferrous ions, and silicates; dissolved organicsubstances such as pesticides, herbicides, plasticizers, styrene monomers, deionization resin material; and colloidal suspensionssuch as silica. While this test method facilit
30、ates the monitoring of these contaminants in high-purity water, in real time, with oneinstrument, this test method is not capable of identifying the various sources of residue contamination or detecting dissolved gasesor suspended particles.5.2 This test method is calibrated using weighed amounts of
31、 an artificial contaminant (potassium chloride). The density ofpotassium chloride is reasonably typical of contaminants found in high-purity water; however, the response of this test method isclearly based on a response to potassium chloride. The response to actual contaminants found in high-purity
32、water may differ fromthe test methods calibration. This test method is not different from many other analytical test methods in this respect.5.3 Together with other monitoring methods, this test method is useful for diagnosing sources of RAE in ultra-pure watersystems. In particular, this test metho
33、d can be used to detect leakages such as colloidal silica breakthrough from the effluent of aprimary anion or mixed-bed deionizer. In addition, this test method has been used to measure the rinse-up time for new liquid filtersand has been adapted for batch-type sampling (this adaptation is not descr
34、ibed in this test method).D5544 1625.4 Obtaining an immediate indication of contamination in high-purity water has significance to those industries usinghigh-purity water for manufacturing components; production can be halted immediately to correct a contamination problem. Theemerging nano-particle
35、technology industry will also benefit from this information.6. Apparatus6.1 The schematic arrangement of the system is shown in Fig. 1. The apparatus is available as a complete instrumentinstru-ment.4.6.2 60 m Filter, 2 60 m Filter, high purity water flows into the apparatus at approximately 120 mL/
36、min and immediatelypasses through a 60 m sintered stainless filter that removes any large debris and then flows to flow controller.6.3 Flow Controller, made of a non-contaminating material such as perfluoroalkoxy (PFA), necessary to supply the nebulizerwith high-purity water at the desired flow rate
37、. The flow controller must contain an air actuated pressure regulator to ensure thatwater is delivered to the nebulizer at a stable flow rate, despite external fluctuations. High-purity water must be delivered to theflow controller and nebulizer through ultra-clean tubes and fittings made from PFA.
38、Nebulizers usually require a very low flowrate, approximately 1 mL/min, for efficient operation. However, such a low flow rate is inadequate for routine monitoring becauseit results in a long response time. This test method is designed to overcome the problem of long response times by using a flowco
39、ntroller to deliver approximately 120 mL/min of high-purity water to the monitoring site and then to divert approximately 14 The sole source of supply of the apparatus known to the committee at this time is Fluid Measurement Technologies, 4106 Hoffman Road, White Bear Lake, MN 55110.If you are aware
40、 of alternative suppliers, please provide this information toASTM International Headquarters. Your comments will receive careful consideration at a meetingof the responsible technical committee 1, which you may attend.FIG. 1 Schematic Diagram of Apparatus Required for This Test MethodD5544 163mL/min
41、 of the flow to the nebulizer through a short tube. This short tube facilitates a short response time. From the pressureregulator, the water flows to the nebulizer through a tee fitting and a section of PFA 500m capillary tubing. The PFA tubinggradually lowers the water pressure and prevents any out
42、-gassing of dissolved gases in the incoming water.6.4 Measuring the Flow Rate, the flow rate of water flowing through the nebulizer is used as an indicator that the NRM 8000is set up and operating correctly. Instead of using a conventional flow meter, the NRM 8000 incorporates a new, patented method
43、of measuring the flow rate. Of the water flowing through the nebulizer, 95% leaves it as part of a waste stream. The waste wateris collected by a weir and stand-pipe system and then delivered as a steady stream of water droplets of identical size.These dropletsfall through a simple light beam.As eac
44、h droplet breaks the beam, a detector senses a scattered light signal, or pulse, and a counterkeeps track of the pulses. An algorithm converts the pulse count to a flowrate (in mL/min.) which is shown on the front paneldisplay.6.5 Nebulizer, required to produce a polydisperse size distribution of dr
45、oplets with a median size of approximately 1 m anda concentration of approximately 107 droplets/s. Within the customed designed nebulizer, the water and compressed air/nitrogen(supplied at a constant flow rate and pressure) combine to form the required stable, poly-dispersed aerosol of ultrapure wat
46、erdroplets. The nebulizer must be supplied with clean, dried filtered compressed air or nitrogen and must be machined from amaterial that will not contaminate the high-purity water. Passivated 316L stainless steel has been used successfully in this testmethod. Details of how to passivate stainless s
47、teel can be found in the Metal Finishing Guidebook.56.6 Heater and Dilution air/nitrogen, the ultrapure water droplets produced by the nebulizer are rapidly heated at 120C. Eachwater droplet is evaporated to dryness, leaving behind a particle of residue consisting of dissolved inorganic material. Ev
48、erynebulizer droplet results in a residue particle: the cleaner the ultrapure water, the smaller the amount of residue within each droplet,and the smaller the resulting residue particle.After the heating, additional compressed air or nitrogen, is introduced from the supplyto prevent re-condensation
49、and to quickly move the residue particles to the Water-based Condensation Particle Counter (WCPC).6.7 Water-based Condensation Particle Counter (WCPC), Thethe WCPC uses a patented technology to count residue particles.Water is used as the working fluid and mixing or adiabatic expansion techniques are not needed. A condensation nucleationtechnique deposits water on the residue particles to grow them to a size that can be detected with a conventional optical countingsystem. The stream of residue particles is uninterrupted and follows a laminar flow
