ANSI/ASHRAE Standard 86-I994 (RA 2006)
`Reafiirmation of ANSI/ASHRAE Standard 86-I994
`
`ASHRAE STAN DARD
`
`Methods of Testing
`the Floc Point
`
`of Refrigeration Grade
`Oils
`
`Approved by the ASHRAE Standards Committee on January 26. 1994, and reatfirmed on January 21, 2006;
`by the ASHRAE Board of Directors on April 19, 1994. and reatiirmed on January 26, 2006; and by the Ameri-
`can National Standards Institute on June 3. 1994. and reaffirmed on January 27. 2006.
`
`ASHRAE Standards are scheduled to be updated on a five-year cyde; the date folowing the standard number
`is the year of ASHRAE Board of Directors approval. The latest copies may be purchased from ASHRAE Cus-
`tomer Service, 1791 Tulie Circle, NE, Attanta. GA 30329-2305. E-mail: ordersflashraeorg. Fax: 404-321-
`5478. Telephone: 404~636-8400 (worldwide) ortoll free 1-800-5274723 (for orders in US and Canada).
`
`0 Copyright 2006 American Society of Heating, Refrigerating and Air-Concitioning Engineers. Inc.
`
`ISSN 1041 -2336
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`K.»-mmmw0'
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`wwmunq
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`American Society of Heating, Refrigerating
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`Arkema Exhibit 1107
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`

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`© American Society of Heating, Refrigerating and Air-Conditioning Engineers, inc. (www.ashrae.org). For personal use only.
`Additional reproduction, distribution, or transmission In either print or digital form is not permitted without ASHRAE's prior written permission.
`
`ASHRAE Standing Standard Project Committee 86
`cognizant TC: TC 3.4, Lubrication
`
`Shelvin Rosen. Chair‘
`Frederick A. Hamm, Secretary
`Thomas D. Annstrong. Jr.‘
`D.F. Hutten|ocher'
`William H. Mapes, Iii‘
`Jose L. Reyes-Gavilan'
`
`Keshav S. Sanvordenker‘
`Carl F. Speich’
`Ganesan Sundaresan'
`Raymond H.P. Thomas‘
`Robert M. wncent‘
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`‘Denotes members of voting status when the document was approved for publication
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`ASHRAE STANDARDS communes 2005-zoos
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`Richard D. Herrnans. Chair
`David E. Knebel, Vice-Chair
`Donald L. Brandt
`Steven T. Bushby
`Paul W Cabot
`Hugh F. Crowther
`Samuel D. Cummings, Jr.
`Robert G. Doerr
`Hakim Elmahdy
`Roger L Hedrick
`John F. Hogan
`Frank E. Jakob
`Stephen D. Kennedy
`
`Jay A. Kohler
`James D. Lutz
`Merle F. McBride
`Mark P. Modera
`Cynis H. Nasseri
`Stephen V. Santoro
`Stephen V. Skalko
`David R. Tree
`Jerry W. White, Jr.
`James E. Woods
`Vifilliam E. Murphy. BOD EXO
`Ronald E. Jarnagin, CO
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`
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` 'p;'4r..ia.<..'«_iSi.-iii=.1Hi;
`
`Claire B. Ramspeck. Assistant Director of Technology for Standards and Special Projects
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`SPECIAL NOTE
`
`This American National Standard (ANS) is a national voluntary consensus standard developed under the auspices of the American
`Society of Heating. Refrigerating and Air-Conditioning Engineers (ASHRAE). Consensus is defined by the American National Standards
`Institute (ANSI). of which ASHRAE is a member and which has approved this standard as an ANS, as “substantial agreement readied by
`directly and materially affected interest categories. This signifies the concurrence of more than a simple majority. but not necessarily unanimity.
`Consensus requires that all views and objections be considered, and that an effort be made toward their resolution.“ Compliance with this
`standard is voluntary until and unless a legal jurisdiction makes compliance mandatory through legislation.
`ASHRAE obtains consensus through participation of its national and international members. associated societies. and public review.
`ASHRAE Standards are prepared by a Project Committee appointed specifically for the purpose of writing the Standard. The Project
`Committee Chair and Vice—Chair must be members of ASHRAE; while other conmlttee members may or may not be ASHRAE members. all
`must be technically qualified in the subject area of the Standard. Every effort is made to balance the concerned interests on all Project
`Committees.
`The Manager of Standards of ASHRAE should be contacted for:
`a. interpretation of the contents of this Standard,
`b. participation in the next review of the Standard.
`c. offering constructive criticism for improving the Standard. or
`d. permission to reprint portions of the Standard.
`
`DISCLAIMER
`
`ASHRAE uses its best efforts to promulgate Standards and Guidelines for the benefit of the public in light of available information and
`accepted industry pradices. However. ASHRAE does not guarantee, certify. or assure the safety or perionnance of any products. components.
`or systems tested, installed. or operated in accordance with ASHRAE's Standards or Guidelines or that any tests conducted under its
`
`Standards or Guidelines will be nonhazardous or free from risk.
`
`
`
`
`ASHRAE Standards and Guidelines are established to assist industry and the pmlic by offering a uniform method of testing for rating
`purposes. by suggesting safe practices in designing and installing equipment, by providing proper definitions of this equipment, and by providing
`
`N I U TRIAL ADVERTISIN 6 P LICY ON STAN ARDS
`
`

`
`© American Society of Heating, Refrigerating and Air-Conditioning Engineers, Inc. (www.ashrae.org). For personal use only.
`Additional reproduction, distribution, or transmission In either print or digital form Is not permitted without ASHRAE’s prior written permission.
`
`CONTENTS
`
`ANSIIASHRAE Standard 86-1994 (RA 2006),
`Methods of Testing the Floc Point of Refrigeration Grade Oils
`
`SECTION
`
`PAGE
`
`Foreword ................................................................................................................................................................. ..2
`
`1 Purpose ........................................................................................................................................................ ..2
`
`2 Scope ........................................................................................................................................................... ..2
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`3 Definition ....................................................................................................................................................... ..2
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`4 Apparatus ..................................................................................................................................................... ..2
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`4.1 Cooling Bath ........................................................................................................................................ ..2
`
`4.2 Temperature-Measuring Devices ........................................................................................................ .. 2
`
`4.3 Sample Tube ....................................................................................................................................... ..2
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`4.4 Metal Connector Fittings ..................................................................................................................... .. 2
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`4.5 Graph Paper........................................................................................................................................ .. 2
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`4.6 Mechanical Vacuum Pump ................................................................................................................. ..2
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`5 Test Procedure ............................................................................................................................................. ..2
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`6 Reproducibility of Results ............................................................................................... .j ............................ ..4
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`7 Significance of Results ................................................................................................................................. .. 4
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`8 References ................................................................................................................................................... ..4
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`Appendix A: Round Robin Test Results ............................................................................................................ ..5
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`Appendix 8: Bibliography .................................................................................................................................. ..5
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`when addenda, interpretations, or errata to this standard have been approved. they can be downloaded
`
`free of charge from the ASHRAE Web site at http:lIwww.eshrae.org.
`
`NOTE
`
`© Copyright 2008 American Society of Heating,
`Refrigerating and Air-Conditioning Engineers, Inc.
`1791 Tullie Circle NE
`Atlanta, GA 30329
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`© American Society of Heating, Refrigerating and Air-Conditioning Engineers, Inc. (www.oshrae.org). For personal use only.
`Additional reproduction, distribution, or transmission in either print or digital form is not perrnltted without ASHRAE’s prior written permission.
`
`(This foreword is not part of this standard. It is merely
`informative and does not contain requirements necessary
`for conformance to the standard.
`It has not been
`
`a
`for
`requirements
`processed according to ANSI
`standard and may contain material that has not been
`subject to public review or a consensus process.)
`
`3. DEFINITION
`
`flocpoint: the highest temperature at which wax or other solid
`substances precipitate when a mixture 10% by volume of oil
`and 90% by volume of R-12 is cooled under specified condi-
`tions.
`
`FOREWORD
`
`4. APPARATUS
`
`This is a reaflirmation of ASHRAE Standard 86-I994.
`This standardfalls under the Standards Committee classifi-
`cation of Standard Method of Measurement. This standard
`was prepared under the auspices ofthe American Society of
`Heating, Refrigerating and A ir-Conditioning Engineers
`(ASHRAE). It may be used, in whole or in part, by an associ-
`ation or government agency with due credit to ASHRAE.
`Adherence is strictly on a voluntary basis and merely in the
`interests of obtaining uniform standards throughout
`the
`industry.
`
`This standard describes a standard test methodfor mea-
`suring thefloc point (waxing tendency) ofrefiigeration grade
`oils. Petroleum-derived lubricating oils are mixtures of large
`numbers ofchemically distinct hydrocarbon molecules. At the
`low temperatures encountered in the low-pressure side of
`refiigeration units, some ofthe larger molecules separatefrom
`the bulk ofthe oil in theform ofwax-like deposits. Wax deposi-
`tion in refrigeration system is undesirable, as wax is known to
`clog capillary tubes and to cause expansion valves to stick The
`floc point procedure requires, in addition to the oil, afluid in
`which the oil is completely miscible with thefluid to a temper-
`ature below that at which floc will form. R-I2 was selected
`because it fits this requirement and it is a commonly used
`refrigerant. R-22, for example, cannot be used because phase
`separation would generally, result before the floc point was
`reached The ensuing hazing, clouding, and separation into
`two dtferent layers precludes obtaining a floc point. The
`industry has a great deal offaith in extrapolating floc point
`datafiom the test tube to field application. History shows this
`faith to bejustified
`
`Development ofafloc point using some otherfluid isfea-
`sible. However,
`it would require a research project, and
`atrapolation of the data fiom anotherfluid without the field
`correlation, which has been availablefor R-l2floc point data,
`could result in majorfieldproblems.
`The changes made for the 2006 reaflirmation were:
`Degree symbols were added to the table in Appendix A.
`
`1. PURPOSE
`
`This standard provides a method for measuring the
`waxing tendency of refrigeration grade oils.
`
`4.] Cooling Bath. A cooling bath suitable for obtaining the
`required temperature can be prepared using dry ice or by
`using a refrigeration system as the cooling source. The cool-
`ing bath should be large enough for testing three sample tubes
`at one time. A large, wide-mouthed, clear dewar flask is sat-
`isfactory. Dry ice in a suitable liquid such as ethanol or ace-
`tone is rccommended. The use of ethanol is preferred because
`this liquid has the advantage of reduced frosting when the
`sample tube is raised from the bath for observation. A
`mechanical stirrer shall be provided for stirring the bath.
`Proper stirring is important to eliminate temperature differ-
`ences. A small piece of aluminum foil in the liquid will indi-
`cate the degree of stirring obtained. If an electric motor is
`used, it should be of a type safe for use above the cooling
`medium. A wire mesh basket with small openings shall be
`provided in the bath forthe introduction ofthe dry ice so small
`pieces of dry ice cannot come into contact with the sample
`tube and cause local cold spots. The wire mesh basket can be
`raised or lowered to control the bath temperature.
`
`4.2 Temperature-Measuring Devices. The temperature is
`measured with a precision electrical digital thermometer, a
`mercury thennometer, or an alcohol thennometer. ASTM
`standard thermometers 6°F or 6°C have been found suitable
`
`for this purpose. For accuracy, thennometers should be peri-
`odically calibrated as covered in ASTM Specification El .1
`
`4.3 Sample Tube. The sample tube consists of a thick-
`walled borosilicate glass tube with a flared end and round bot-
`tom, as shown in Figure 1. Tube dimensions are 0.375 in. (9.5
`mm) ID X 0.600 in. (15 mm) OD X 9 in. (228 mm) long. The
`tube shall be permanently graduated at the 10.0 mL volume
`(calibrated at room temperature).
`
`4.4 Metal Connector Fittings. The metal connector fittings
`shall be as shown in Figure l.
`
`In certain instances, graph paper is used
`4.5 Graph Paper.
`with a glass plate to judge the cloudiness of the test sample.
`The graph should have 20 lines per 1.0 in. (25.4 mm).
`
`4.6 Mechanical Vacuum Pump. A mechanical vacuum
`pump suitable for obtaining an absolute pressure of 0.1 mm
`Hg shall be used.
`
`2. SCOPE
`
`5. TEST PROCEDURE
`
`The test for floc point is intended to detennine the waxing
`tendency of refrigeration grade oils at low temperatures. The
`test is based on evaluation ofthe wax precipitation tendency of
`a mixture containing 90% R-12 and 10% by volume ofthe oil
`
`5.] Use proper safety precautions, such as a face mask,
`safety shield, and heavy gloves, when handling the charged
`pressure tube outside the cooling bath or when evacuating the
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`

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`© American Society of Heating, Refrigerating and Air-Conditioning Engineers, Inc. (www.ashrae.org). For personal use only.
`Additional reproduction, distribution, or transmission in either print or digital form is not permitted without ASHRAE's prior written permission.
`
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`L25 IIEX.
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`ADAPTER
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`TEFLON GASKET OR
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`ALL DIMENSIONS
`IN INCHES.
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`.375
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`.600 TUBE DI A.
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`

`
`© American Society of Heating, Refrigerating and Air-Conditioning Engineers, Inc. (www.ashrae.org). For personal use only.
`Additional reproduction, distribution, or transmission in either print or digital form is not permitted without ASHRAE's prior written permission.
`
`to prevent fire. These solvents and their vapors are very flam-
`mable.
`
`uum or heating the oil in an open container in an oven at 302°F
`(150°C) for about one hour.
`
`The glass tube should not be used at a pressure exceeding
`80 psig (552 kPa) or temperature exceeding 200°F (93°C). The
`tube must not be subjected to any bending strain. Glass
`components should be periodically inspected for signs of
`wear. Erosion, stress, cracks, nicks, or deep scratches provide
`early warning for glass replacement. The glass may erode
`evenly so wear is not visibly noticeable. Ifwear is detected, the
`component should be replaced to eliminate the potential cause
`of breakage.
`
`5.2 Prepare the equipment. The sample tube shall be
`cleaned, dried, and stored in a desiccator prior to use. Appro-
`priate precautions shall be taken to eliminate the introduction
`ofwater into the sample tube while charging with oil or refrig-
`erant. Prepare a suitable manifold or other system for evacu-
`ating and charging the sample tube. The refrigerant tubing
`shall be dried before use.
`
`5.3 Assemble the cooling bath. Make sure that stirring of
`the liquid is adequate for continuous transfer, both vertically
`and horizontally, within the cooling bath. Install the thennom-
`eter to be used in a test tube immersed in the bath and till this
`
`test tube with the same fluid used in the cooling bath.
`
`5.4 Transfer 1.0 mL of the sample oil into the sample glass
`tube using a 2.0 mL syringe for precise oil measurement (at
`room temperature). Attach a small brass valve to the sample
`tube using the metal connector fittings. Evacuate the sample
`tube to about 0.] mm Hg absolute pressure to de-gas the oil.
`
`Introduce a quantity of liquid R-12 so that the total vol-
`ume of oil and R-l2 is 10.0 mL. The method of introduction
`
`shall preclude the introduction of water into the tube. This
`addition of R-l2 and the measurement of the volume shall be
`
`done in the cooling bath at a temperature of —25°F to —30°F
`(—32°C to —34°C).
`
`5.6 The tube shall be disconnected from the charging
`assembly and allowed to warm up to the point where the oil-
`refrigerant mixture may be made homogenous by shaking.
`CAUTION: Follow safety precautions. Any excess Refrig-
`erant-12 can then be bled off at a temperature above —20°F
`(—29°C). In this way, the volume of the refrigerant-oil mix-
`ture can be adjusted to 10.0 ml. when measured at —25°F to
`—30°F (—32°C to —34°C).
`
`5.7 The sample tube containing the refrigerant-oil mixture
`shall then be immersed in the cooling bath, which has previ-
`ously been adjusted to a temperature of approximately O°F
`(—l8°C). Then the temperature of the cooling bath shall be
`lowered at a rate of l°F to 2°F (l/2°C to 1°C) per minute by
`careful addition of dry ice. Temperature readings with the
`thermometer or thermocouple in the test tube in the bath give
`values comparable to the temperature in the test sample tube.
`
`If an oil shows a cloud at O°F (—l 8°C), the test shall be
`
`5.9 The tube shall be observed as the temperature is lowered
`beginning at O°F (—l8°C). If a clear dewar flask is used, the
`tube may be viewed through the dewar flask. The tube may
`also be removed briefly (10 seconds) from the cooling bath
`for viewing. Avoid disturbing the contents by removing the
`tube carefully without shaking. When distinct flocculant
`material is observed in the mixture, the test thennometer in
`the bath shall be read. This temperature shall be reported as
`the floc point. Some oils show a haze at temperatures 5°F to
`10°F (3°C to 6°C) above the actual floc point.
`
`In some instances, the mixture becomes increasingly
`5.10
`hazy or cloudy as the temperature is lowered but does not
`fonn distinct flocculant material. When this occurs, the tube
`shall be removed from the cooling bath and held against a
`glass plate with graph paper (see 4.5) behind the glass plate.
`When the cloudiness in the tube prevents seeing the lines on
`the graph paper, then the temperature shall be read, and this
`condition shall be considered an endpoint to the floc point
`test. If desired, the tube may be warmed up and the test
`repeated using the same sample tube.
`
`5.1] Repeat the test with a second oil sample, run at a dif-
`ferent time. If the results of these two observations agree
`within 5°F (3°C), the average of the two shall be reported as
`the floc point of the oil.
`
`6. REPRODUCIBILITY OF RESULTS
`
`Duplicate detenninations of floc point by the same oper-
`ator in the same laboratory should agree within 5°F (3°C).
`Duplicate detenninations between two different laboratories
`should be considered suspect if they differ by more than 15°F
`(8°C). These reproducibility results are based on a round robin
`test conducted in 1982 by seven laboratories using three oil
`samples (see Appendix A). The results were evaluated using
`the “ASTM Suggested Recommended Practice for Conduct-
`ing an lnterlaboratory Test Program to Detemiine the Preci-
`sion of Test Methods” (l977).2
`
`7. SIGNIFICANCE OF RESULTS
`
`The floc point can be used to compare the waxing tenden-
`cies of different oils. In actual refrigeration systems, diflerent
`refrigerants and oil concentrations are encountered, so test
`results cannot be used to directly predict actual system perfor-
`mance. The oil concentration in the expansion devices of most
`refrigeration and air-conditioning systems is considerably
`lower than 10% by volume, resulting in a significantly lower
`temperature at which wax will separate from the refrigerant-
`oil mixture.
`
`8. REFERENCES
`
`l. ASTM. I992. ASTM Specification El-92, StandardSpec-
`ificarionfor AS?‘M Thermometers.
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`
`© American Society of Heating, Refrigerating and Air-Conditioning Engineers, Inc. (www.ashrae.org). For personal use only.
`Additional reproduction, distribution, or transmission in either print or digital form is not permitted without ASHRAE's prior written permission.
`
`(This appendix is not part of this standard. It is merely informative and does not contain requirements necessary for
`confonnance to the standard. It has not been processed according to the ANSI requirements for a standard and may
`contain material that has not been subject to public review or a consensus process. Unresolved objectors on informative
`material are not offered the right to appeal at ASHRAE or ANSI.)
`
`_
`
`APPENDIX A
`
` _::
`Test Conducted June 1932'
`
`FLOC romr °r
`noc romr °c
`
`on 3
`
`40 450
`
`-67 455
`
`-73 -72
`
`-43 -49
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`-so -58
`
`-42 -3s
`
`on A
`
`-70 -70
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`-67 -59
`
`_
`
`on B
`
`—5l -51
`
`.54 .55
`
`-ss -53
`
`on c
`
`-44 -45
`
`-46 -so
`
`-41 -39
`
`-47 -44
`
`-77 -32 4|
`
`-48 -52 -52
`
`-41 -3s -43
`
`—6l -as -63
`
`-44 -47 -47
`
`-41 -39 -42
`
`-so -79 -so
`
`-57 -so -as
`
`-39 -39 -40
`
`42 -62 -62
`
`-so -49 -49
`
`-39 -39 -4o
`
`-91 -37
`
`-60 -55
`
`-45 -44
`
`-52 -43
`—
`‘ Data developed by project committee members for the I983 edition ofttus standard.
`
`-68 -56
`
`-60 -so
`
`-51 -4s
`
`_
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`-43 -42
`
`
`
`(This appendix is not part of this standard. It is merely informative and does not contain requirements necessary for
`conformance to the standard. It has not been processed according to the ANSI requirements for a standard and may
`contain material that has not been subject to public review or a consensus process. Unresolved objectors on informative
`material are not offered the right to appeal at ASHRAE or ANSI.)
`
`APPENDIX B
`
`BIBLIOGRAPHY
`
`Deutsche Normen DIN-51351, Testing ofLubricants: Determination ofFIoc Point ofRefiigerator Oils.
`Deutsche Normen DIN-51590 Part 2, Determination of the R-I2 lnsolubles Content of Refrigeration 0ils—Procedure at
`40°C.
`'
`
`“Kinetic” Technical Bulletin 14, Handling ‘Freon’ Fluorinated Hydrocarbon Compounds in the Laboratory, Freon Products
`Div., E. I. DuPont de Nemours & Co.
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`© American Society of Heating, Refrigerating and Air-Conditioning Engineers, Inc. (www.ashrae.org). For personal use only.
`Additional reproduction, distribution, or transmission in either print or digital form is not permitted without A$HRAE's nnor written pemiission.
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`© American Society of Heating, Refrigerating and Air-Conditioning Engineers, Inc. (www.ashrae.org). For personal use only.
`Additional reproduction, distribution, or transmission in either print or digital form is not permitted without ASHRAE’s prior written permission.
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`POLICY STATEMENT DEFINING ASI-IRAE'S CONCERN
`FOR THE ENVIRONMENTAL IMPACT OF ITS ACTIVITIES
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`ASHRAE is concerned with the impact of its members’ activities on both the indoor and outdoor environment. ASHRAE's
`members will strive to minimize any possible deleterious effect on the indoor and outdoor environment of the systems and
`components in their responsibility while maximizing the beneficial effects these systems provide. consistent with accepted
`standards and the practical state of the art.
`ASHRAE's short-range goal is to ensure that the systems and components within its scope do not impact the indoor and
`outdoor environment to a greater extent than specified by the standards and guidelines as established by itself and other
`responsible bodies.
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`through its Standards Committee and extensive technil committee structure,
`As an ongoing goal, ASHRAE will,
`continue to generate up-to-date standards and guidelines where appropriate and adopt, recommend. and promote those new
`and revised standards developed by other responsible organizations.
`Through its Handbook. appropriate chapters will contain up-to-date standards and design considerations as the material is
`systematically revised.
`ASHRAE will take the lead with respect to dissemination of environmental information of its primary interest and will seek
`out and disseminate infomiation from other responsible organizations that is pertinent, as guides to updating standards and
`guidelines.
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`The effects of the design and selection of equipment and systems will be considered within the scope of the system's
`intended use and expected misuse. The disposal of hazardous materials, if any. will also be considered.
`ASHRAE's primary concern for environmental
`impact will be at the site where equipment within ASHRAE's scope
`operates. However, energy source selection and the possible environmental impact due to the energy source and energy
`transportation will be considered where possible. Recommendations conoeming energy source selection should be made by
`its members.
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`© American Society of Heating, Refrigerating and Air-Conditioning Engineers, Inc. (www.ashrae.org). For personal use only.
`Additional reproduction, distribution, or transmission in either print or digital form is not permitted without ASHRAE’s prior written permission.
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`About ASHRAE
`
`is an
`The American Society of Heating. Refrigerating and Air-Conditioning Engineers (ASHRAE), founded in 1894.
`international organization of some 50,000 members. ASHRAE fulfills its mission of advancing heating, ventilation, air
`conditioning. and refrigeration to serve humanity and promote a sustainable world through research, standards writing,
`publishing, and continuing education.
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`For more information or to become a member of ASHRAE. visit www.ashrae.org.
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`To stay current with this and other ASHRAE standards and guidelines, visit www.ashrae.org/standards.
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`ASHRAE has two collections of standards and guidelines available on CD that include one year of unlimited access to
`download monthly updates. including addenda. errata. and interpretations. ASHRAE Standards and Guidelines contains
`the complete library, and Essential Standards contains ASHRAE's 12 most referenced standards and guidelines. Both
`include the User’s Manuals for Standard 90.1 and Standard 62.1. For more information on these products, visit the
`Standards and Guidelines section of the ASHRAE bookstore atwww.ashrae.org/bookstore.
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`IMPORTANT NOTICES ABOUT THIS STANDARD
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`sustainable use of resources.
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`To ensure that you have all of the approved addenda, errata, and interpretations for this
`standard, visit www.ashrae.orgIstandards to download them free of charge.
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`Addenda, errata, and interpretations for ASHRAE standards and guidelines will no longer
`be distributed with copies of the standards and guidelines. ASHRAE provides these
`addenda, errata, and interpretations only in electronic fonn in order to promote more
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