FDUS 1689

FINAL DRAFT UGANDA

STANDARD First Edition
2017-mm-dd

Standard Test Method for Distillation Range of Volatile Organic

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Liquids

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Reference number
FDUS 1689: 2017

This Final Draft Uganda Standard, FDUS 1689: 2017, Standard Test Method for
Distillation Range of Volatile Organic Liquids, is based on ASTM D1078 − 11, Standard
Test Method for Distillation Range of Volatile Organic Liquids, Copyright ASTM
International, 100 Barr Harbor Drive, West Conshohocken, PA 19428, USA, pursuant to
license with ASTM International © UNBS 2017
FDUS 1689: 2017

Compliance with this standard does not, of itself confer immunity from legal obligations

A Uganda Standard does not purport to include all necessary provisions of a contract. Users are
responsible for its correct application

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© UNBS 2017
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All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilised in any
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form or by any means, electronic or mechanical, including photocopying and microfilm, without prior written
permission from UNBS.

Requests for permission to reproduce this document should be addressed to

The Executive Director

Uganda National Bureau of Standards
P.O. Box 6329
Kampala
Uganda
Tel: +256 417 333 250/1/2/3
Fax:+ 256 414 286 123
E-mail: [email protected]
Web: www.unbs.go.ug

This Final Draft Uganda Standard, FDUS 1689: 2017, Standard Test Method for Distillation Range of Volatile
Organic Liquids, is based on ASTM D1078 − 11, Standard Test Method for Distillation Range of Volatile
Organic Liquids, Copyright ASTM International, 100 Barr Harbor Drive, West Conshohocken, PA 19428, USA,
pursuant to license with ASTM International

ii © UNBS 2017 - All rights reserved

 FDUS 1689: 2017

National foreword

Uganda National Bureau of Standards (UNBS) is a parastatal under the Ministry of Trade, Industry and
Cooperatives established under Cap 327, of the Laws of Uganda, as amended. UNBS is mandated to co-
ordinate the elaboration of standards and is
(a) a member of International Organisation for Standardisation (ISO) and

(b) a contact point for the WHO/FAO Codex Alimentarius Commission on Food Standards, and

(c) the National Enquiry Point on TBT Agreement of the World Trade Organisation (WTO).

The work of preparing Uganda Standards is carried out through Technical Committees. A Technical

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Committee is established to deliberate on standards in a given field or area and consists of representatives of
consumers, traders, academicians, manufacturers, government and other stakeholders.

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Draft Uganda Standards adopted by the Technical Committee are widely circulated to stakeholders and the

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general public for comments. The committee reviews the comments before recommending the draft standards
for approval and declaration as Uganda Standards by the National Standards Council.
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This Final Draft Uganda Standard, FDUS 1689: 2017, Standard Test Method for Distillation Range of Volatile
Organic Liquids, is based on ASTM D1078 − 11, Standard Test Method for Distillation Range of Volatile
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Organic Liquids, Copyright ASTM International, 100 Barr Harbor Drive, West Conshohocken, PA 19428, USA,
pursuant to license with ASTM International.
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This standard was developed by the Chemicals and Environment Standards Technical committee, (UNBS/TC
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5)

Wherever the words, “ASTM Standard" appear, they should be replaced by "Uganda Standard."
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© UNBS 2017 - All rights reserved iii

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.

Designation: D1078 − 11

Designation: 195/98

Standard Test Method for

Distillation Range of Volatile Organic Liquids1
This standard is issued under the fixed designation D1078; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.

1. Scope* responsibility of the user of this standard to establish appro-

1.1 This test method covers the determination of the distil- priate safety and health practices and determine the applica-
lation range of liquids boiling between 30 and 350°C, that are bility of regulatory limitations prior to use. Specific hazard
statements are given in Section 7.

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chemically stable during the distillation process, by manual or
automatic distillation procedures.

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2. Referenced Documents
1.2 This test method is applicable to organic liquids such as 2.1 ASTM Standards:2

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hydrocarbons, oxygenated compounds, chemical D86 Test Method for Distillation of Petroleum Products at
intermediates, and blends thereof. Atmospheric Pressure

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1.3 The values stated in SI units are to be regarded as E1 Specification for ASTM Liquid-in-Glass Thermometers
standard. No other units of measurement are included in this E29 Practice for Using Significant Digits in Test Data to
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standard. Determine Conformance with Specifications
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1.4 For purposes of determining conformance of an ob- E133 Specification for Distillation Equipment
served or a calculated value using this test method to relevant E299 Test Method for Trace Amounts of Peroxides In
Organic Solvents
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specifications, test result(s) shall be rounded off “to the nearest

unit” in the last right-hand digit used in expressing the 2.2 ASTM Adjuncts:
specification limit, in accordance with the rounding-off method Determination of Precision and Bias for Use in Test
Methods for Petroleum Products and Lubricants3
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of Practice E29.
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1.5 For hazard information and guidance, see the supplier’s 3. Terminology
Material Safety Data Sheet. 3.1 Definitions:
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1.6 Warning—Mercury has been designated by EPA and 3.1.1 initial boiling point, n—the temperature indicated by
many state agencies as a hazardous material that can cause
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the distillation thermometer at the instant the first drop of

central nervous system, kidney and liver damage. Mercury, or condensate leaves the condenser tube.
its vapor, may be hazardous to health and corrosive to
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3.1.2 dry point, n—the temperature indicated at the instant

materials. Caution should be taken when handling mercury and the last drop of liquid evaporates from the lowest point in the
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mercury-containing products. See the applicable product Ma- distillation flask, disregarding any liquid on the side of the
terial Safety Data Sheet (MSDS) for details and EPA’s website flask.
(http://www.epa.gov/mercury/faq.htm) for additional informa-
3.1.3 decomposition point, n—the thermometer reading that
tion. Users should be aware that selling mercury or mercury-
coincides with the first indications of thermal decomposition of
containing products, or both, in your state may be prohibited by
the liquid in the flask.
state law.
1.7 This standard does not purport to address all of the 3.2 Definitions of Terms Specific to This Standard:
safety concerns, if any, associated with its use. It is the 3.2.1 final boiling point, n—the maximum thermometer
reading obtained during the test.

1 2
This test method is under the jurisdiction of ASTM Committee D01 on Paint For referenced ASTM standards, visit the ASTM website, www.astm.org, or
and Related Coatings, Materials, and Applications and is the direct responsibility of contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Nov. 15, 2011. Published December 2011. Originally the ASTM website.
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approved in 1949. Last previous edition approved in 2005 as D1078 – 05. DOI: Available from ASTM International Headquarters. Order Adjunct No.
10.1520/D1078-11. ADJD6300.

*A Summary of Changes section appears at the end of this standard

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
Copyright by ASTM Int'l (all rights reserved); Tue Jan 31 05:09:48 EST 2017
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 D1078 − 11
3.2.1.1 Discussion—This usually occurs after the evapora- those obtained when using gas heat. (See Section 9 for factors
tion of all liquid from the bottom of the flask. The term that cause superheating, and Appendix X1 for a discussion on
“maximum temperature” is a frequently used synonym. the use of electric heaters.)
3.2.2 end point 5 minutes, n—the thermometer reading 6.4 Distillation Receiver:
obtained 5 min after the 95 % distillation point if no dry or final 6.4.1 Manual Distillation Receiver—A 100-mL cylinder
boiling point occurs. graduated in 1 mL subdivision and having an overall height of
250 to 260 mm.
4. Summary of Test Method 6.4.2 Automatic Distillation Receiver—A receiver to be
4.1 A 100-mL specimen is distilled under conditions equiva- used with automatic distillation in accordance with the instru-
lent to a simple batch differential distillation. The temperature ment manufacturer’s instructions, conforming to the dimen-
of the thermometer is equilibrated with that of the refluxing sions given in 6.4.1, with the exception of the graduations.
liquid before the distillate is taken over. Boiling temperatures 6.4.2.1 Automatic Distillation Level Follower—The level
observed on a partial immersion thermometer are corrected to follower/recording mechanism of the automatic apparatus shall
standard atmospheric pressure to give true boiling tempera- have a resolution of 0.1 mL with an accuracy of 61 mL.
tures. 6.5 Temperature Measurement Devices:
6.5.1 Manual Distillation Thermometers—Partial immer-
5. Significance and Use sion thermometers as listed in Table 1, conforming to Speci-

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5.1 This test method provides a method of measurement of fication E1. Other liquid-in-glass thermometers or temperature
distillation range of volatile organic liquids. The relative measuring devices that provide equivalent range, accuracy, lag

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volatility of organic liquids can be used with other tests for time and precision may be used. Both bore corrections and
either ice or steam standardization corrections are recom-

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identification and measurement of quality. Therefore, this test
method provides a test procedure for assessing compliance mended as appropriate.
with a specification. 6.5.2 Automatic Distillation Temperature Sensors—

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Temperature measurement systems using thermocouples or
5.2 This test method also provides an empirical value of
resistance thermometers shall exhibit the same temperature lag
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residue, solvent recovery capacity, and loss (or non-recovery)
and accuracy as the appropriate and calibrated mercury-in-
on heating. Organic liquids are used as solvents in many
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glass thermometer. Confirmation of the calibration of these

chemical processes. As the relative volatility, residual matter
temperature sensors shall be done at regular intervals. This can
and recovery capability affect the efficiency of these processes,
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be accomplished potentiometrically by the use of standard

this test method is useful in manufacturing control.
precision resistance, depending on the type of probe. Another
technique is to distill pure toluene (99.9 + % purity) and
6. Apparatus
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compare the temperature indicated by the thermocouple or

6.1 Distillation Apparatus—See Condenser and Cooling
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resistance thermometer with that shown by the mercury-in-

Bath section, Apparatus Assembly Using Gas Burner figure, glass thermometer.
Apparatus Assembly Using Electric Heater figure, and Metal
NOTE 2—Toluene is shown in reference manuals as boiling at 110.6°C
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Shield or Enclosure for Flask section of Specification E133.

(corrected for barometric pressure) under the conditions of a manual
6.1.1 Manual Distillation Apparatus—See Condenser Cool-
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D1078 distillation that uses a partial immersion thermometer.

ing Bath section, Apparatus Assembly Using Gas Burner
figure, Apparatus Assemble Using Electric Heater figure, and
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Metal Shield or Enclosure for Flask section of Specification

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E133. TABLE 1 Thermometers

6.1.2 Automated Distillation Apparatus—Any automated ASTM Sub-
instrument that complies with 6.2-6.5, and is capable of Thermometer IP Range, °C division,
Number °C
achieving the operating parameters given in 9.1.3 and 9.1.4, is
2CA 62CA −5 to + 300 1.0
acceptable. 3CA 73CA −5 to + 400 B

6.2 Distillation Flasks, 200-mL of borosilicate glass com- 14C ... 38 to 82 0.1
37C 77C −2 to + 52 0.2
plying with the specifications given in Distillation Flask 38C 78C 24 to 78 0.2
section, Fig. 3, and Flask C of Specification E133. 39C 79C 48 to 102 0.2
40C 80C 72 to 126 0.2
NOTE 1—Liquid superheating in a new flask may be prevented by 41C 81C 98 to 152 0.2
depositing a small amount of carbon in the bottom of the flask. This may 42CA 82CA 95 to 255 0.5
be accomplished by heating and decomposing a pinch of tartaric acid in 102C 83C 123 to 177 0.2
the bottom of the flask. The flask is then prepared for use by washing with 103C 84C 148 to 202 0.2
water, rinsing with acetone, and drying. 104C 85C 173 to 227 0.2
105C 86C 198 to 252 0.2
6.3 Source of Heat—An adjustable gas burner or electric 106C 87C 223 to 277 0.2
107C 88C 248 to 302 0.2
heater so constructed that sufficient heat can be obtained to
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distill the product at the uniform rate specified in Section 8. For These thermometers have more temperature lag than the other thermometers
listed herein and are not satisfactory for use with narrow-boiling range liquids.
narrow-range (less than 2°C) liquids, an electric heater may be B
1 to 301°C; 1.5°C above 301°C.
used only if it has been proven to give results comparable to

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 D1078 − 11
7. Hazards 8.1.5 Adjust the temperature of the appropriate portion of
7.1 Warning—Certain solvents and chemical intermedi- the sample to the applicable temperature shown in Table 2.
ates, particularly, but not only ethers and unsaturated com- 8.2 Automatic Distillation Apparatus—For assembly of au-
pounds, may form peroxides during storage. These peroxides tomatic distillation apparatus, consult instrument manufactur-
may present a violent explosion hazard when the chemical is er’s operating manual.
distilled, especially as the dry point is approached. When
peroxide formation is likely because of chemical type or length 9. Procedure
of storage, the material should be analyzed for peroxides (See
Test Method E299.) and if they exist in hazardous concentra- 9.1 Manual Distillation Procedure:
tions, appropriate precautions should be taken such as destroy- 9.1.1 Using the graduated receiver measure 100 6 0.5 mL
ing the peroxide before distillation, shielding, or destroying the of the temperature-adjusted sample. Remove the flask from the
sample and not running the test. apparatus and transfer the fresh specimen directly to the flask,
allowing the graduate to drain for 15 to 20 s.
7.2 Most organic solvents and chemical intermediates will
burn. In the operation of the distillation apparatus, use a NOTE 6—For viscous liquids, a longer drainage period may be
suitable catch pan and shielding to contain spilled liquid in the necessary to complete the transfer of the specimen to the flask, but the
drainage time should not exceed 5 min. Do not allow any of the specimen
event of accidental breakage of the distillation flask. to enter the vapor tube.
7.3 Provide adequate ventilation to maintain solvent vapor 9.1.2 Connect the flask to the condenser by inserting the

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concentrations below the lower explosive limit in the immedi- vapor tube of the flask into the condenser, making a tight
ate vicinity of the distillation apparatus, and below the thresh-

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connection with a well-rolled cork or similar material. Adjust
old limit value in the general work area. the position of the heat shield so that the neck of the flask is

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8. Preparation of Apparatus vertical and the vapor tube extends into the condenser tube a
distance of 25 to 50 mm. Have the bottom of the flask resting

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8.1 Manual Distillation Apparatus: firmly in the hole of the heat shield. Insert the thermometer as
8.1.1 Clean and dry the condenser tube by swabbing with a IC described in 8.1.2. Place the receiver, without drying, at the
piece of soft lint-free cloth attached to a wire or cord, or by any outlet of the condenser tube in such a position that the
other suitable means. condenser tube extends into the graduate at least 25 mm but
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8.1.2 Use the thermometer listed in the material specifica- does not extend below the 100-mL mark. If the initial boiling
tion for the product under study. If no thermometer is specified, point of the material is below 70°C, immerse the cylinder in a
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select one from Table 1 with the smallest graduations that will transparent bath and maintain at a temperature of 10 to 20°C
cover the entire distillation range of the material. Preferably, an throughout the distillation. Place a flat cover on the top of the
equivalent non-mercury thermometer should be used if avail-
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graduate to prevent condensed moisture from entering the

able. Center the thermometer into the neck of the flask through graduate.
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a tight-fitting cork stopper so that the upper end of the

9.1.3 A certain amount of judgment is necessary in choosing
contraction chamber (or bulb if Thermometer 2C or IP ther-
the best operating conditions to get acceptable accuracy and
mometer 62C is used) is level with the lower side of the vapor
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precision for materials having different distilling temperatures.

tube at its junction with the neck of the flask. (See Apparatus
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As a general guide, it is recommended that:

Assembly Using Gas Burner figure of Test Method D86.)
9.1.3.1 For materials having an initial boiling point below
NOTE 3—It is far more important that the bulb and contraction chamber 150°C, the following conditions be established:
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be immersed in the refluxing zone than that the immersion mark on the (a) Heat Shield—Hole size, 32-mm diameter.
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thermometer be placed at any specific point.

(b) Heating Rate—Time from application of heat to first
8.1.3 Position the correct heat shield (see 9.1.3.1 and drop of distillate, 5 to 10 min, and time of rise of vapor column
9.1.3.2). in neck of flask to side arm, 21⁄2 to 31⁄2 min.
NOTE 4—For low-boiling materials, cool the apparatus to room tem- 9.1.3.2 For materials having an initial boiling point above
perature before starting the test. 150°C, the following conditions should be established:
8.1.4 Fill the condenser bath with water of the appropriate (a) Heat Shield—Hole size, 38-mm diameter.
temperature shown in Table 2. (b) Heating Rate—Time from application of heat to first
drop of distillate, 10 to 15 min, and time of rise of vapor
NOTE 5—When distilling pure compounds always ensure that the
column in neck of flask to side arm, sufficiently rapid to permit
condenser bath temperature is above the crystallizing point of the
compound. collection of the first drop of distillate within 15 min of the start
of heating.
TABLE 2 Temperatures 9.1.4 Adjust the heat input so that the distillation proceeds at
Initial Boiling Condenser, Sample, a rate of 4 to 5 mL/min (approximately 2 drops per second),
Point,°C °C °C and move the receiving cylinder so that the tip of the condenser
Below 50 0 to 3 0 to 3 tube touches one side of the cylinder after the first drop falls
50 to 70 0 to 10 10 to 20 (initial boiling point). Record the readings of the distillation
70 to 150 25 to 30 20 to 30
Above 150 35 to 50 20 to 30 thermometer after collecting 5, 10, 20, 30, 40, 50, 60, 70, 80,
90, and 95 mL of distillate.

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 D1078 − 11
9.1.5 Without changing the heater setting, continue distilla- 10.2.2 Use a board that is free of cracks and checks.
tion beyond the 95 % point until the dry point is observed. 10.2.3 Set the flask snugly in the hole in the upper insulating
Record the temperature at this point as the dry point (Section board.
3). If a dry point is not obtained (that is, if active decomposi- 10.3 Application of Heat—Attention should be given to
tion should occur before the dry point is reached, as evidenced burner placement, position, and character of flame, as follows:
by a rapid evolution of vapor or heavy fumes; or if there is 10.3.1 Apply the source of heat directly beneath the flask.
liquid remaining on the bottom of the flask when the maximum Any variation would result in heating a larger portion of
temperature is observed on the distillation thermometer), surrounding air to a higher temperature than that of the flask.
record this fact. 10.3.2 The flame should not have a larger cross section than
9.1.6 When a dry point cannot be obtained, report as the end is necessary, and should be nonluminous.
point the maximum temperature observed on the distillation 10.3.3 Place the burner at a level such that the complete
thermometer or final boiling point (Section 3). When active combustion area of a nonluminous flame is approximately 3⁄4
decomposition is encountered, the rapid evolution of vapor and in. (20 mm) below the board.
heavy fumes is usually followed by a gradual decrease in the
distillation temperature. Record the temperature and report as 10.4 Extraneous Heat Source—An extraneous source of
the decomposition point (Section 3). If the expected drop in heat such as sunlight falling directly on the flask can cause
temperature does not occur, record the maximum temperature superheating.
observed on the distillation thermometer 5 min after the 95 % 10.5 Condition of Equipment—Observe caution in employ-

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point has been reached, and report as “end point, 5 min.” This ing the apparatus for immediate reuse. For low-boiling mate-
notation shows that a true end point could not be reached rials, cool the heating unit to room temperature before starting

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within the given time limit. In any event, the end point should the test.

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not exceed 5 min after the 95 % point. 10.6 Use of Electric Heaters—Electric heaters generally
9.1.7 Read and record the barometric pressure. cause superheating. These should be used only after they have
9.1.8 After the condenser tube has drained, read the total

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been proven to give results comparable to those obtained when
volume of distillate and record it as recovery. The total yield of IC using gas heat. The superheating effect obtained from electric
distillate from a material having a distillation range of 10°C or heaters may be minimized, but not completely eliminated, by
less should be not less than 97 % for nonviscous liquids. For selecting a heater that, by its design, concentrates the heating
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viscous liquids and materials having a wider distillation range elements to a minimum area, and contains a minimum amount
than 10°C, a yield of 95 volume % is satisfactory. If yields are of ceramic material in its overall construction. The fulfillment
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not obtained within these limits, repeat the test. of these requirements will reduce, but not completely elimi-
9.1.9 If any residue is present, cool to room temperature and nate, the amount of extraneous heat radiating around the
pour into a small cylinder graduated in 0.1-mL subdivisions.
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perimeter of the heat resistant board on which the distillation

Measure the volume and record it as residue. Record the flask is placed.4 (See Appendix X1 for a more complete
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difference between 100 and the sum of the residue plus discussion of the problems encountered in the use of electric
recovery as distillation loss. heaters.)
9.2 Automatic Distillation Procedure:
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9.2.1 Using the automatic distillation receiver measure 100 11. Calculations
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6 0.5 mL of the temperature-adjusted sample. Transfer the 11.1 Manual Distillation Calculations:
fresh specimen directly to the flask, allowing the receiver to 11.1.1 Thermometer Bore Correction—Apply the correc-
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drain for 15 to 20 s (see Note 6). tions for any variations in the bore of the thermometer as given
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9.2.2 Connect the distillation flask to the condenser and fit by the calibration.
the temperature measuring device to the flask according to the 11.1.2 Thermometer Bulb Shrinkage Correction—Apply the
instrument manufacturer’s instruction. correction for shrinkage of the mercury bulb of the thermom-
9.2.3 Start the distillation following the instrument manu- eter as determined by any change in its ice or steam point
facturer’s instruction. where applicable. Other means can be employed, such as the
use of a platinum-resistance thermometer or a National Bureau
10. Factors Causing Superheating of Standards thermometer.
10.1 In general, any condition whereby the temperature 11.1.3 Barometer Pressure Correction—After applying the
surrounding the vapor exceeds the temperature of the vapor in corrections for thermometer error, correct each reading for
equilibrium with the liquid will cause superheating. Specific deviation of the barometric pressure from normal by adding
factors conducive to superheating are as follows, and should be algebraically the correction calculated as follows:
avoided: 11.1.3.1 For values of K in degrees Celsius per millimetre of
10.2 Flame in Contact with the Flask—The applied gas mercury
flame should be prevented from contacting more than the
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specified portion of the flask by the following procedures: The sole source of supply of the Lo-Cap heater known to the committee at this
time is Precision Scientific Co., Chicago, IL. If you are aware of alternative
10.2.1 Maintain the correct overall dimensions and speci-
suppliers, please provide this information to ASTM International Headquarters.
fied hole diameter of the heat resistant board. The hole must be Your comments will receive careful consideration at a meeting of the responsible
perfectly circular, with no irregularities. technical committee,1 which you may attend.

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 D1078 − 11
Correction 5 K ~ 760 2 P ! (1) 11.1.4 If the overall distillation range of the sample does not
exceed 2°C, combined thermometer (bore irregularities and
11.1.3.2 For values of K in degrees Celsius per millibar:
bulb shrinkage) and barometric corrections may be made on
Correction 5 K ~ 1013 2 P ! (2) the basis of the difference between the observed 50 % boiling
where: point and the true boiling point at 760 mm as given in Table 3.
K = rate of change of boiling point with pressure, in degrees 11.2 Automatic Distillation Calculations—
Celsius per millibar, as given in Table 3 (Note 7), and Barometric correction shall be done according to 11.1.3 and
11.1.4.
P = barometric pressure in millibars at standard tempera-
ture and pressure. 12. Report
NOTE 7—For other pure compounds not listed in Table 3, the value K
12.1 Report the results in a manner conforming with the
should be obtained from the literature. For narrow-boiling hydrocarbon specifications of the material tested. If no definite manner of
materials, the value of K may be assumed as 0.00012 times the normal reporting is specified, report the corrected temperatures at each
boiling point on the absolute temperature scale. observed volume, and report the volume percentages of resi-
due, recovery, and distillation loss.

TABLE 3 Change of Boiling Point with Pressure 13. Precision and Bias
5,6

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Value of K, °C K, °C per Boiling Point 13.1 Interlaboratory Study:
Compound per mm Hg at mbar at at 760 mm Hg,
Boiling Point Boiling Point °C 13.2 The precision of this test method was obtained from an

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Acetone 0.039 0.029 56.1 interlaboratory study conducted in 2000 involving manual and

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n-Amyl alcohol 0.041 0.031 138.0
n-Amyl acetate 0.048 0.036 149.5
automatic distillation procedures. The study involved six
Aromatic solvent 0.049 0.037 ... samples of different boiling point ranges, done in duplicate.
naphtha Ten laboratories did automatic D1078 distillation, and five

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Benzene 0.043 0.032 80.1
IC laboratories did manual D1078 distillation. It was found that
Isobutyl acetate 0.045 0.035 117.3 the precision is dependent on the boiling point temperature.
n-Butyl acetate 0.045 0.035 126.1 The data were statistically evaluated using the D2PP3 software
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sec-Butyl acetate 0.045 0.034 112.4

Isobutyl alcohol 0.036 0.027 107.9
available from ASTM.
n-Butyl alcohol 0.037 0.028 117.7 13.3 Repeatability—Two results, each the mean of two runs,
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sec-Butyl alcohol 0.035 0.026 99.5

obtained by the same operator should be considered suspect if
Diacetone alcohol 0.050 0.037 ... they differ by more than the repeatability values shown in
Diethylene glycol 0.050 0.037 245.0 Tables 4 and 5 at a 95 % confidence level.
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Dipropylene glycol 0.051 0.038 232.8

13.4 Reproducibility—Two results, each the mean of two
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Ethyl acetate 0.041 0.030 77.2

Ethyl alcohol 0.033 0.025 78.3
runs, obtained by operators in different laboratories should be
Ethylene glycol 0.045 0.033 197.6 considered suspect if they differ by more than the reproduc-
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2-Butoxyethanol 0.047 0.035 171.2 ibility values shown in Tables 4 and 5 at a 95 % confidence
2-Ethoxyethanol 0.044 0.033 135.1
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2-Ethoxyethyl acetate 0.046 0.035 156.3

level.
13.5 Bias:
Hexylene glycol 0.045 0.033 197.1
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n -Hexyl acetate 0.050 0.037 171.6 13.5.1 Absolute Bias—Since the temperature measuring de-
vices specified by this test method are calibrated against the
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Isophorone 0.057 0.043 215.3 normal boiling point of toluene (99.9+ % purity), this test
Methyl alcohol 0.033 0.025 64.5 method has no bias with respect to pure toluene as a reference
Methyl ethyl ketone 0.043 0.032 79.6 material.
Methyl isoamyl acetate 0.048 0.036 146.2 13.5.2 Relative Bias Between Manual and Automatic D1078
Methyl isoamyl ketone 0.048 0.036 144.9
Methyl isobutyl 0.041 0.030 131.8 Distillation—Statistical comparison between the variances of
carbinol automatic and manual D1078 distillation results did not indi-
Methyl isobutyl ketone 0.046 0.035 116.2 cate any statistically significant difference. Statistical compari-
Perchloroethylene 0.048 0.036 121.2 son of the averages of the six samples used in the study
Isopropyl alcohol 0.033 0.025 82.3 indicated that the paired-sample, two-tailed, t-test for the initial
Isopropyl acetate 0.041 0.030 88.5
boiling point (IBP) and 50 % distillation point showed a small
Propylene glycol 0.043 0.032 187.6
Pyridine 0.046 0.035 115.4 relative bias that is not statistically significant. A small but
statistically significant bias was indicated for the automatic and
Toluene 0.046 0.035 110.6
Trichloroethylene 0.043 0.032 87.1
manual D1078 dry point (DP). Table 6 gives a summary of the

Vinyl acetate 0.040 0.030 72.7

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Supporting data have been filed at ASTM International Headquarters and may
Xylene (mixed 0.049 0.037 ... be obtained by requesting Research Report RR:D01-1114.
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isomers) Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D01-1123.

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 D1078 − 11
TABLE 4 Summary of D1078 Precision Data, °C
Parameter Manual D1078 Automatic D1078
Repeatability, r Reproducibility, R Repeatability, r Reproducibility, R
IBP 0.00528 X 0.0107 X 0.00450 X 0.0156 X
50 % 0.00471 X 0.00647 X 0.00209 X 0.00683 X
DP 0.00684 X 0.01301 X 0.00396 X 0.01070 X
Boiling range 0.0405 (X + 5) 0.1163 (X + 5) 0.0445 (X + 5) 0.1294 (X + 5)

where X = the mean of two results being compared.

TABLE 5 Sample Calculation of D1078 Precision Values, °C

Manual D1078 RR—IBP Data Auto D1078 RR—IBP Data
IBP r R IBP r R
50 0.3 0.5 50 0.2 0.8
75 0.4 0.8 75 0.3 1.2
100 0.5 1.1 100 0.5 1.6
125 0.7 1.3 125 0.6 2.0
150 0.8 1.6 150 0.7 2.3
175 0.9 1.9 175 0.8 2.7

Manual D1078 RR—50 % Data Auto D1078 RR—50 % Data

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50 % r R 50 % r R
50 0.2 0.3 50 0.1 0.3

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75 0.4 0.5 75 0.2 0.5
100 0.5 0.6 100 0.2 0.7

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125 0.6 0.8 125 0.3 0.9
150 0.7 1.0 150 0.3 1.0
175 0.8 1.1 175 0.4 1.2

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Manual D1078 RR—DP Data Auto D1078 RR—DP Data
DP r R DP r R
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50 0.3 0.7 50 0.2 0.5
75 0.5 1.0 75 0.3 0.8
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100 0.7 1.3 100 0.4 1.1

125 0.9 1.6 125 0.5 1.3
150 1.0 2.0 150 0.6 1.6
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175 1.2 2.3 175 0.7 1.9

Manual D1078 RR—BPRA Data Auto D1078 RR—BPR Data

BPR r R BPR r R
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0.5 0.2 0.6 0.5 0.2 0.7

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5 0.4 1.2 5 0.4 1.3

10 0.6 1.7 10 0.7 1.9
15 0.8 2.3 15 0.9 2.6
20 1.0 2.9 20 1.1 3.2
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25 1.2 3.5 25 1.3 3.9

30 1.4 4.1 30 1.6 4.5
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BPR = boiling point range.
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relative bias observed for the samples used in the study. The method. If an agreement on which method to designate cannot be made,
observed bias (if any) are only for the samples studied and may the referee test method will be the manual method.
not be necessarily applicable to other samples.
14. Keywords
NOTE 8—In cases of dispute, the parties involved may agree to
designate either the manual or the automatic method to be the referee test 14.1 distillation range; solvents

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 D1078 − 11
TABLE 6 Relative Bias (Auto–Manual) for D1078 Distillation, °C
Sample Initial Boiling Point 50 % B.P. Dry Point
Auto Manual Auto Manual Auto Manual
Toluene 110.19 110.16 110.61 110.54 110.67 110.71
Commercial nonene 136.31 136.07 137.72 137.68 142.49 142.25
Special cut naphtha 167.99 167.25 170.98 170.16 179.05 178.63
Light naphtha 98.26 98.05 101.66 101.65 114.76 114.03
Naphtha 118.47 118.24 126.03 125.59 144.73 144.02
Mineral spirits 162.13 160.40 172.71 171.65 193.11 192.71
Relative Bias Relative Bias Relative Bias
Toluene 0.03 0.07 −0.04
Commercial nonene 0.24 0.04 0.24
Special cut naphtha 0.74 0.82 0.42
Light naphtha 0.21 0.01 0.73
Naphtha 0.23 0.44 0.71
Mineral spirits 1.73 1.06 0.40

Average relative bias 0.53 0.41 0.41

F–test (95 % confidence) Equivalent Equivalent Equivalent
t–test (95 % confidence) Equivalent Equivalent Not equivalent

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APPENDIX

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(Nonmandatory Information)

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X1. DISCUSSION ON THE USE OF ELECTRIC HEATERS WHEN APPLYING TEST METHOD D1078/IP 195 TO THE DETER-

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MINATION OF THE DISTILLATION RANGE OF NARROW RANGE (<2°C) PURE COMPOUNDS IC
X1.1 Test Method D1078/IP 195, in the hands of a compe- the distillation flask which in turn is due to the relatively large
tent operator using properly designed equipment, has been
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area of the distillation board exposed to the heating elements of

found over the years to be a valuable tool in detecting the the electric heater. For example, the heating elements of the
presence of low-boiling and high-boiling impurities in rela- electric heater4 cover an area of 63.5 by 76 mm whereas the
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tively pure compounds. flame of a properly adjusted gas burner can be concentrated to
an area no larger than the 32-mm hole of the supporting heat
X1.2 In recent years many laboratories, for reasons of safety
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resistant (or ceramic) board. This means that when the heating
and convenience, have eliminated the availability of natural or elements of the electric heater are brought up to sufficient
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artificial gas, with the resulting trend toward the exclusive use
temperature to effect the proper distillation rate of the metha-
of electric heaters in place of gas burners. The use of electricity
nol, a relatively large area of the board also is exposed to the
instead of gas as the source of heat, coupled with the
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heat of these elements so that as the end of the distillation is

application of this test method to materials of extremely high
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approached, a considerable amount of heat is being radiated

purity and narrow distillation ranges (2°C or less), has resulted
from the board to the air surrounding the distillation flask. This
in the distortion of the dry point. This distortion effect can be
hot air surrounding the flask is sufficient to cause a distortion of
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illustrated by comparing the distillation range results using gas

the dry point as the last drop of liquid is vaporized from the
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and electric heat on a sample of high-purity methanol (Table

bottom of the flask. Conversely, the ability to concentrate the
X1.1). The purity of the methanol employed was established by
gas chromatography and other instrumental procedures. gas flame to only the 32-mm exposed area of the flask
minimizes the extent of the extraneous heat radiating from the
X1.3 The higher dry point obtained with the electric heater board, which, in turn, eliminates the distortion of the dry point
is due to the large amount of extraneous heat radiating around from this cause. This conclusion was substantiated by results
from the following experiment: The board with the 32-mm
TABLE X1.1 Comparison of Gas Versus Electric Heat hole was replaced by a 190.7 by 190.7-mm stainless steel plate
Electric in which a 32-mm hole had been cut. Four turns of 6.4-mm
Gas Heat
HeaterA copper tubing with sufficient inlet and outlet leads were
Range Range silver-soldered to the underside of the plate so that water could
Determination 1: be circulated through the tubing during the course of the
Initial boiling point 64.5 0.3 64.5 1.5 distillation. With this “water-cooled board” substituted for the
Dry point 64.8 66.0
Determination 2: standard board, only the heat from the electrical elements
Initial boiling point 64.5 0.4 64.5 1.9 immediately under the 32-mm outlet could reach the distilla-
Dry point 64.9 66.4 tion flask. The heat emanating from the outer perimeter of the
Mean range ... 0.35 ... 1.7
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heater was dissipated by the water circulating through the
The sole source of supply of the Lo-Cap heater known to the committee at this
time is Precision Scientific Co. tubing on the underside of the board, as evidenced by the
ability to hold one’s finger on top of the“ water-cooled board”

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 D1078 − 11
during the course of the distillation. Using the same high-purity and in the other case, the specially prepared “black bottom”
methanol employed in the previous experiment, distillation 200-mL flask was employed. Both of these special conditions
ranges were determined using gas heat, electric heat, and were compared to the standard procedure using gas heat. The
electric heat with the “water-cooled board” substituted for the results of this experiment, given in Table X1.3, show that the
standard board. These results are given in Table X1.1. use of the “black-bottom flask” in conjunction with the electric
heater and “water-cooled board” causes a significant lowering
X1.4 The results from the above experiment demonstrate of the dry point which confirms the theory that infrared
the effect the extraneous radiant heat from the electric heater radiation emanating from the electric heating elements causes
had on the dry point, and also suggest a means whereby this a slight distortion of the dry point.
effect could be greatly reduced.
X1.6 The above discussion and experimental evidence are
X1.5 Despite the fact that the use of a “water-cooled board” presented to show how and why the use of electric heater
in conjunction with an electric heater eliminated the extraneous causes a distortion of the dry point when carrying out the
radiant heat surrounding the distillation flask, it is evident from procedure as specified in Test Method D1078/IP 195. Although
the results in Table X1.2 that the dry point obtained when using this distortion is of a minor nature, and therefore of little
the electric heater and “water-cooled board” was still signifi- importance when applying this test method to compounds or
cantly higher than the dry point obtained when using gas heat. mixtures which have distillation ranges of 5°C or more, the
The assumption was made that this “residual” interference to effect becomes significant when the method is applied to
the dry point was caused by infrared radiation from the

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narrow range (2°C or less) pure compounds. It is the further
glowing electric heating elements. This assumption has been objective of this discussion to suggest to those laboratories

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supported by the following experimental evidence: The bottom equipped with only electricity, a technique whereby the distil-
of a standard 200-mL distillation flask was coated with a lation range results obtained with electric heaters may be made

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38-mm diameter circle of black ceramic marking ink. The equivalent to those obtained with gas heat.
black ink was in turn fired into the glass by heating the bottom

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of the flask to a dull-red heat with a gas-oxygen glass X1.7 The sponsoring subcommittee of this test method has
blowtorch. The presence of this black coating on the bottom of not had the opportunity to apply this technique to a sufficiently
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the flask would absorb any infrared radiation emanating from large number of compounds over a wide range of boiling
the electrical heating elements, thus preventing it from affect- temperatures to warrant including it as a part of Test Method
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ing the bulb of the thermometer at the end of the distillation. D1078/IP 195; and is, therefore, presenting it for information
Distillation ranges were then determined on the same methanol purposes only. Comments are solicited from those attempting
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as used in the previous experiments following Test Method to employ the suggestions contained in this report as well as
D1078/IP 195, except that in one case a standard 200-mL flask other ideas that might be employed to equate the use of electric
was used with an electric heater plus the “water-cooled board,”
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heat with gas heat.

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TABLE X1.2 Comparison of Electric Heat Plus Water-Cooled Board to Gas Heat

Gas Heat Electric HeatA Electric HeatA plus

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Water-Cooled Board
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Range Range Range

Determination 1:
Initial boiling point 64.5 0.3 64.5 1.6 64.5 0.5
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Dry point 64.8 66.1 65.0

Determination 2:
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Initial boiling point 64.6 0.3 64.5 1.4 64.5 0.6

Dry point 64.9 65.9 65.1
Mean range ... 0.3 ... 1.5 ... 0.55
A
The sole source of supply of the Lo-Cap heater known to the committee at this time is Precision Scientific Co.

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 D1078 − 11
TABLE X1.3 Effect of Infrared Radiation on Dry Point
Electric HeaterA with Water-Cooled Electric HeaterA with Water-Cooled
Gas Heat Board and Standard Flask Board and Black-Bottom Flash
Range Range Range
Determination 1:
Initial boiling point 64.5 0.3 64.5 0.6 64.6 0.2
Dry point 64.8 65.1 64.8
Determination 2:
Initial boiling point 64.5 0.4 64.6 0.6 64.6 0.2
Dry point 64.9 65.2 64.9
Mean range ... 0.35 ... 0.6 ... 0.25
A
The sole source of supply of the Lo-Cap heater known to the committee at this time is Precision Scientific Co.

SUMMARY OF CHANGES

Committee D01 has identified the location of selected changes to this standard since the last issue (D1078 - 05)

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that may impact the use of this standard. (Approved November 15, 2011.)

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(1) Added warning regarding the use of mercury in Section 1. throughout the standard, and replaced it with liquid-in-glass
(2) Removed reference to mercury-in-glass thermometer thermometer or temperature measuring device, as required.

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ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned

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in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.
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This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
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if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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make your views known to the ASTM Committee on Standards, at the address shown below.

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 FDUS 1689
FINAL DRAFT UGANDA
STANDARD First Edition
2017-mm-dd

Standard Test Method for Distillation Range of Volatile Organic

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Liquids

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Reference number
FDUS 1689: 2017

This Final Draft Uganda Standard, FDUS 1689: 2017, Standard Test Method for
Distillation Range of Volatile Organic Liquids, is based on ASTM D1078 − 11, Standard
Test Method for Distillation Range of Volatile Organic Liquids, Copyright ASTM
International, 100 Barr Harbor Drive, West Conshohocken, PA 19428, USA, pursuant to
license with ASTM International © UNBS 2017
FDUS 1689: 2017

Compliance with this standard does not, of itself confer immunity from legal obligations

A Uganda Standard does not purport to include all necessary provisions of a contract. Users are
responsible for its correct application

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© UNBS 2017
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All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilised in any
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form or by any means, electronic or mechanical, including photocopying and microfilm, without prior written
permission from UNBS.

Requests for permission to reproduce this document should be addressed to

The Executive Director

Uganda National Bureau of Standards
P.O. Box 6329
Kampala
Uganda
Tel: +256 417 333 250/1/2/3
Fax:+ 256 414 286 123
E-mail: [email protected]
Web: www.unbs.go.ug

This Final Draft Uganda Standard, FDUS 1689: 2017, Standard Test Method for Distillation Range of Volatile
Organic Liquids, is based on ASTM D1078 − 11, Standard Test Method for Distillation Range of Volatile
Organic Liquids, Copyright ASTM International, 100 Barr Harbor Drive, West Conshohocken, PA 19428, USA,
pursuant to license with ASTM International

ii © UNBS 2017 - All rights reserved

 FDUS 1689: 2017

National foreword

Uganda National Bureau of Standards (UNBS) is a parastatal under the Ministry of Trade, Industry and
Cooperatives established under Cap 327, of the Laws of Uganda, as amended. UNBS is mandated to co-
ordinate the elaboration of standards and is
(a) a member of International Organisation for Standardisation (ISO) and

(b) a contact point for the WHO/FAO Codex Alimentarius Commission on Food Standards, and

(c) the National Enquiry Point on TBT Agreement of the World Trade Organisation (WTO).

The work of preparing Uganda Standards is carried out through Technical Committees. A Technical

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Committee is established to deliberate on standards in a given field or area and consists of representatives of
consumers, traders, academicians, manufacturers, government and other stakeholders.

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Draft Uganda Standards adopted by the Technical Committee are widely circulated to stakeholders and the

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general public for comments. The committee reviews the comments before recommending the draft standards
for approval and declaration as Uganda Standards by the National Standards Council.
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This Final Draft Uganda Standard, FDUS 1689: 2017, Standard Test Method for Distillation Range of Volatile
Organic Liquids, is based on ASTM D1078 − 11, Standard Test Method for Distillation Range of Volatile
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Organic Liquids, Copyright ASTM International, 100 Barr Harbor Drive, West Conshohocken, PA 19428, USA,
pursuant to license with ASTM International.
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This standard was developed by the Chemicals and Environment Standards Technical committee, (UNBS/TC
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5)

Wherever the words, “ASTM Standard" appear, they should be replaced by "Uganda Standard."
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