1、Designation: D 5544 05Standard Test Method forOn-Line Measurement of Residue After Evaporation of High-Purity Water1This standard is issued under the fixed designation D 5544; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the yea
2、r of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of dissolvedorganic and inorganic matter and colloidal material found
3、inhigh-purity water used in the semiconductor, and relatedindustries. This material is referred to as residue after evapo-ration (RAE). The range of the test method is from 0.01g/L(ppb) to 20 mg/L (ppm).1.2 This test method uses a continuous, real time monitoringtechnique to measure the concentratio
4、n of RAE. A pressurizedsample of high-purity water is supplied to the test methodsapparatus continuously through ultra-clean fittings and tubing.Contaminants from the atmosphere are therefore preventedfrom entering the sample. General information on the testmethod and a literature review on the cont
5、inuous measurementof RAE has been published.21.3 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility
6、of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. For specific hazardsstatements, see Section 8.2. Referenced Documents2.1 ASTM Standards:3D 1129 Terminology Relating to WaterD 2777 Practice for
7、 Determination of Precision and Bias ofApplicable Methods of Committee D19 on WaterD 3370 Practices for Sampling Water from Closed ConduitsD 3864 Guide for Continual On-line Monitoring Systemsfor Water AnalysisD 3919 Practice for Measuring Trace Elements in Water byGraphite Furnace Atomic Absorption
8、 SpectrophotometryD 5127 Guide for Ultra Pure Water Used in the Electronicsand Semiconductor IndustryE 1184 Practice for Electrothermal (Graphite Furnace)Atomic Absorption Analysis3. Terminology3.1 DefinitionsFor definitions of terms used in this testmethod, refer to Terminology D 1129.3.2 Definitio
9、ns of Terms Specific to This Standard:3.2.1 aerosol, nany solid or liquid particles, with anominal size range from 10 nm to 100 m, suspended in a gas(usually air).3.2.2 colloidal suspension, nany material in suspension(for example, silica) with a nominal particle size less than 100nm.3.2.3 condensat
10、ion particle counter (CPC), ninstrumentfor detecting very small aerosol particles in a size range fromapproximately 10 nm to 2 to 3 m. The CPC cannot differen-tiate between particles of varying size within this size range; itreports the number of particles with a size greater than thatdefined by its
11、 detection efficiency curve. Detection is indepen-dent of particle composition.3.2.4 detection effciency, nin this test method, detectionefficiency represents a curve relating particle size to a countersability to detect that size.3.2.5 diffusion screen, na fine mesh screen used to filterresidue par
12、ticles of a particular size.3.2.6 high-purity water, nwithin the context of this testmethod, high-purity water is defined as water containingresidue after evaporation in the range from 0.1 g/L to 20mg/L.3.2.7 polydisperse, adja size population, in this case ofaerosol particles, composed of many diff
13、erent sizes; the oppo-site of monodisperse, a distribution of just one size.1This test method is under the jurisdiction of ASTM Committee D19 on Waterand is the direct responsibility of Subcommittee D19.03 on Sampling of Water andWater-Formed Deposits, Analysis of Water for Power Generation and Proc
14、ess Use,On-Line Water Analysis, and Suveillance of Water.Current edition approved Jan. 1, 2005. Published January 2005. Originallyapproved in 1994. Last previous edition approved in 2004 as D 5544 94 (2004).2Blackford, D. B., and Kerrick, T. A., Proceeding of Microcontamination 91,San Jose, CA, 1991
15、, pp. 3951. Published by Canon Communications Inc., 3340Ocean Park Blvd., Suite 1000, Santa Monica, CA 90405.3For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the sta
16、ndards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.2.8 realtime, nthe time that an event is occurring plusthe response time; in this case, the response time is 3 to 5 min.Therefore, cont
17、amination is recorded 3 to 5 min after it occurs.3.2.9 residue after evaporation, ncontaminants remainingafter 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 arepre
18、sentative sample of high-purity water from a pressurizedsupply line (refer to Practices D 3370, Practice C on ContinualSampling, and Practice D 3864). The temperature of theincoming high-purity water should ideally be at room tempera-ture, but not more than 50C. The high-purity water issubsequently
19、cooled to a constant temperature of 18C. Anatomizer is supplied with the cooled high-purity water at aconstant 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, theatomizer p
20、roduces a polydisperse size distribution of dropletswith a median size of approximately 1 m, and a concentrationof approximately 107droplets/s, or 1012droplets/mL4.2 The droplets enter a drying column; are rapidly mixedwith dried, filtered, heated (normally at 120C) compressed air,or nitrogen; and d
21、ried within the first few centimetres of thedrying column. The temperature of the drying column can beset at lower temperatures (95, 70, or 45C) if informationconcerning the dissolved organic fraction of residue is re-quired. Each atomizer droplet produces a particle of nonvola-tile residue. As the
22、residue particles emerge from the dryingcolumn, a small percentage is removed and passed through adiffusion screen before being counted by a condensationparticle counter (CPC). Different combinations of diffusionscreens modify the detection efficiency of the CPC, allowingdetection in the 0.1-g/L to
23、20-mg/L range.4.3 The CPC works as follows: The residue particles enter asaturator and pass through a heated, volatile liquid-soakedwick. The wick dips into the liquid reservoir and continuallydraws up liquid through an inclined tube. The liquid evaporatesand saturates the aerosol stream with vapor.
24、 N-butyl alcoholhas been used successfully as the volatile liquid in this testmethod. The vapor-saturated aerosol passes into a verticalcondenser tube, cooled by a thermoelectric device. The vaporcools, becomes super-saturated, and begins to condense on theparticle nuclei to form large droplets that
25、 can then be countedwith a relatively simple optical particle counter. A moreelaborate description of the CPCs method for distinguishingbetween clean and dirty water is described in Appendix X1.4.4 A calibration technique (described in detail in Section10) uses concentration standards of high-purity
26、 potassiumchloride (KCl) to convert the CPC count concentration inparticles per cubic centimetre into RAE concentration inmicrograms per litre or milligrams per litre.Agraphite furnaceatomic absorption spectrometer (GFAAS) can be used to checkthe concentration of KCl in this test method standard (se
27、ePractices D 3919 and E 1184).5. Significance and Use5.1 Even so-called high-purity water will contain contami-nants. While not always present, these contaminants maycontribute one or more of the following: dissolved active ionicsubstances such as calcium, magnesium, sodium, potassium,manganese, amm
28、onium, bicarbonates, sulfates, nitrates, chlo-ride and fluoride ions, ferric and ferrous ions, and silicates;dissolved organic substances such as pesticides, herbicides,plasticizers, styrene monomers, deionization resin material;and colloidal suspensions such as silica. While this test methodfacilit
29、ates the monitoring of these contaminants in high-puritywater, in real time, with one instrument, this test method is notcapable of identifying the various sources of residue contami-nation or detecting dissolved gases or suspended particles.5.2 This test method is calibrated using weighed amounts o
30、fan artificial contaminant (potassium chloride). The density ofpotassium chloride is reasonably typical of contaminants foundin high-purity water; however, the response of this test methodis clearly based on a response to potassium chloride. Theresponse to actual contaminants found in high-purity wa
31、termay differ from the test methods calibration. This test methodis not different from many other analytical test methods in thisrespect.5.3 Together with other monitoring methods, this testmethod is useful for diagnosing sources of RAE in ultra-purewater systems. In particular, this test method can
32、 be used todetect leakages such as colloidal silica breakthrough from theeffluent of a primary anion or mixed-bed deionizer. In addition,this test method has been used to measure the rinse-up time fornew liquid filters and has been adapted for batch-type sampling(this adaptation is not described in
33、this test method).5.4 Obtaining an immediate indication of contamination inhigh-purity water has significance to those industries usinghigh-purity water for manufacturing components; productioncan be halted immediately to correct a contamination problem.The biomedical and power-generating industries
34、 will alsobenefit from this information.6. Apparatus6.1 The schematic arrangement of the system is shown inFig. 1. The apparatus is available as a complete instrument4.6.2 Flow Controller, made of a non-contaminating materialsuch as perfluoroalkoxy (PFA), necessary to supply the atom-izer with high-
35、purity water at the desired flow rate. The flowcontroller must contain a pressure regulator to ensure thatwater is delivered to the atomizer at a stable flow rate, despiteexternal fluctuations. High-purity water must be delivered tothe flow controller and atomizer through ultra-clean tubes andfittin
36、gs made from PFA polytetrafluor-oethylene. Atomizersusually require a very low flow rate, approximately 1 mL/min,for efficient operation. However, such a low flow rate isinadequate for routine monitoring because it results in a long4The sole source of supply of the apparatus known to the committee a
37、t this timeis Fluid Measurement Technologies, 4225 White Bear Parkway, Suite 1225, VadnaisHeights, MN 55110. If you are aware of alternative suppliers, please provide thisinformation to ASTM International Headquarters. Your comments will receivecareful consideration at a meeting of the responsible t
38、echnical committee1, whichyou may attend.D5544052response time. This test method is designed to overcome theproblem of long response times by using a flow controller todeliver approximately 70 mL/min of high-purity water to themonitoring site and then to divert 1 mL/min of the flow to theatomizer th
39、rough a short tube. This short tube facilitates a shortresponse time.6.3 Cooling Block, necessary to cool the water and maintainit at a stable temperature before it enters the atomizer (18C isadequate). The cooling block incorporates a thermoelectricdevice capable of maintaining the cooling block at
40、 the requiredtemperature.6.4 Atomizer, required to produce a polydisperse size dis-tribution of droplets with a median size of approximately 1 mand a concentration of approximately 107droplets/s. Theatomizer must be supplied with clean, dried filtered com-pressed air or nitrogen and must be machined
41、 from a materialthat will not contaminate the high-purity water. Passivated 316stainless steel has been used successfully in this test method.Details of how to passivate stainless steel can be found in theMetal Finishing Guidebook.56.5 Mixing Chamber and Drying Column, for mixing thewater droplets f
42、rom the atomizer with dried, heated (at 120Cor, if required, 95, 70, or 45C) dilution air or nitrogen. Thewater droplets and dilution air pass through a drying columnthat evaporates all of the water from the droplets. The residuefrom each droplet is left as a particle. A drying columnapproximately 2
43、.5 cm in diameter and 30 cm in length hasworked well in this test method, with a ratio of dilution air toatomizer air of approximately 10:1.6.6 Diffusion ScreensFifty-millimetre diameter diffusionscreens made of a fine stainless steel wire cloth used to shift thedetection efficiency of the CPC to la
44、rger sizes. Wire cloth witha wire diameter of 25 m and a square weave opening of 38 m(referred to as a 400 mesh in the Tyler equivalent designation)has worked well in this test method.6.7 Condensation Particle Counter (CPC), containing asaturator, condenser, and optical particle counter to enlarge t
45、heparticles to a uniform size and count them in particles per cubiccentimetre. The flow rate through the CPC is 2.8 L/min.6.7.1 Inside the saturator is a wick soaked in a volatileliquid.The wick dips into a liquid reservoir and draws up liquidcontinually through an inclined tube. The liquid evaporat
46、es andsaturates the aerosol stream with vapor.6.7.2 The vapor-saturated aerosol passes into a verticalcondenser tube, cooled by a thermoelectric device. Aerosolparticles of a certain size and above (nominally 10-nm diam-eter) act as nucleation sites upon which the vapor can condenseto form droplets
47、(nominally 10-m diameter). Droplets passfrom the condenser tube through a nozzle into the opticaldetector.6.7.3 The CPCs focusing optics consist of a laser diode andbeam-shaping optics. This combination forms a beam of laserlight above the aerosol exit nozzle. The sensors collecting5Metal Finishing
48、Guidebook, Elsevier Science, New York, NY, 60th ed., 1992.FIG. 1 Schematic Diagram of Apparatus Required for This Test MethodD5544053optics collect the light scattered by the droplets and focus thislight onto a low-noise photo-detector.7. Reagents and Materials7.1 Purity of ReagentsReagent grade che
49、micals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society wheresuch specifications are available.6Other grades may be used,provided 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 WaterUnless otherwise indicated, referenceto water shall be understood to mean Electronic and Semicon-ductor grade water Type E
