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Thank you for interesting in our services. We are a non-profit group that run this website to share documents. We need your ast to maintenance this website. Please help us to share our service with your friends. D — 01 Designation: A number in parentheses indicates the year of last reapproval. A superscript epsilon e indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 7.
Summary of Test Method 4. The temperature of the mercury in the ast, is equilibrated with that of the refluxing liquid before the distillate is taken over. Boiling temperatures observed on a partial immersion thermometer are corrected to standard atmospheric pressure to give true boiling temperatures. Significance and Use 5.
HDA 620: Distillation Analyzer
The relative volatility of organic liquids can be used with other tests for identification and measurement of quality. Therefore, this test method provides a test procedure for v1078 compliance with a specification.
Organic liquids are used as solvents in many chemical processes. As the relative volatility, residual matter and recovery capability affect the efficiency of these processes, this test method is astmm in manufacturing control. Current edition approved June 10, Originally published as D — 49 T.
Last previous edition D — Confirmation of the calibration of these temperature sensors shall be done at regular intervals.
This can be accomplished potentiometrically by the use of standard precision resistance, depending on the type of probe. Another technique is to distill pure toluene NOTE 1—Liquid superheating in a new flask may be prevented by depositing a small amount of carbon in the bottom of the flask.
This may be accomplished by heating and decomposing a pinch of tartaric acid in the bottom of the flask. The flask is then prepared for use by washing with water, rinsing with acetone, and drying. NOTE 2—Toluene is shown in reference manuals as boiling at See Section 9 for factors that cause superheating, and Appendix X1 for a discussion on the use of electric heaters.
Both bore corrections and either ice or steam standardization corrections are recommended. These peroxides may present a violent explosion hazard when the chemical is distilled, especially as the dry point is approached.
When peroxide formation is likely because of chemical type or length of storage, the material should be analyzed for peroxides See Test Method E In the operation of the distillation apparatus, use a suitable catch pan and shielding to contain spilled liquid in the event of accidental breakage of the distillation flask.
Preparation of Apparatus 8. If no thermometer is specified, select one from Table 1 with the smallest graduations that will cover the entire distillation range of the material. Center the thermometer into the neck of the flask through a tight-fitting cork stopper so that the upper end of the contraction chamber or bulb if Thermometer 2C or IP thermometer 62C is used is level with the lower side of the vapor tube at its junction with the neck of the flask.
NOTE 4—For low-boiling materials, cool the apparatus to room temperature before starting the test. A These thermometers have more temperature lag than the other thermometers listed herein and are not satisfactory for use with narrow-boiling range liquids. Record the readings of the distillation thermometer after collecting 5, 10, 20, 30, 40, 50, 60, 70, 80, 90, and 95 mL of distillate.
Record the temperature at this point as the dry point Section 3.
If a dry point is not obtained that is, if active decomposition awtm occur before the dry point is reached, as evidenced by a rapid evolution of vapor or heavy fumes; or if there is liquid remaining on the bottom of the flask when the maximum temperature is observed on the distillation thermometerrecord this fact. When active decomposition is encountered, the rapid evolution of vapor and heavy fumes is usually followed by a gradual decrease in the distillation temperature.
Record the temperature and report as the decomposition point Section 3. If yields are not obtained within these limits, repeat the test. Measure the volume and record it as residue. Record the axtm between and the sum of the residue plus recovery as distillation loss. Transfer the fresh specimen directly to the flask, allowing the receiver to drain for 15 to 20 s see Note 6. Remove the flask from the apparatus and transfer the fresh specimen directly to the flask, allowing the graduate to drain for 15 to 20 s.
NOTE 6—For viscous liquids, a longer drainage period may be necessary to complete the transfer of the specimen to the flask, but the drainage time should not exceed qstm min.
Do not allow any of the specimen to enter the vapor tube. Adjust the position of the heat shield so that the neck of the flask is vertical and the vapor tube extends into the condenser tube a distance of 25 to 50 mm. Have the bottom of the flask resting firmly in the hole of the heat shield. Insert the thermometer as described in 8.
Asgm the receiver, without drying, at the outlet of the condenser tube in such a position that the condenser tube extends into the graduate at least 25 mm but does not extend below the mL mark. Place a flat cover on the top of the graduate to prevent condensed moisture from entering the graduate.
As a general guide, it is recommended that: Factors C1078 Superheating Specific 3 D factors conducive to superheating are as follows, and should be avoided: The hole must be perfectly circular, with no irregularities.
Any variation would result in heating zstm larger portion of surrounding air to a higher temperature than that of the flask. For low-boiling materials, cool the heating unit to room asym before starting the test. These should be used only after they have been proven to give results comparable to those obtained when using gas heat. The superheating effect obtained from electric heaters may be minimized, but not completely eliminated, by selecting a heater that, by its design, concentrates the heating elements to a minimum area, and contains a minimum amount of ceramic material in its overall construction.
The fulfillment of these requirements will reduce, but not completely eliminate, the d078 of extraneous heat radiating around the perimeter of the asbestos-cement board on which the distillation flask is placed. Other means can be employed, such as the use of a platinum-resistance thermometer or a National Bureau of Standards thermometer.
ASTM D – 11 Standard Test Method for Distillation Range of Volatile Organic Liquids
Compound 6 The sole source of supply of the Lo-Cap heater known to the committee at this time is Precision Scientific Co. Your comments will receive careful consideration at a meeting of the responsible technical committee,1 which you may attend. IBP 50 75 r 0. For narrow-boiling hydrocarbon materials, the value of K may be assumed as 0.
If no definite manner of reporting is specified, 1d078 the corrected temperatures at each observed volume, and report the volume percentages of residue, recovery, and distillation loss. Precision and Bias The study involved adtm samples of different boiling point ranges, done in duplicate.
Ten laboratories did automatic D distillation, and five laboratories did manual D distillation.
PAC-Lab Instruments-ASTM D
It was found that the precision is dependent on the boiling point temperature. A small but statistically significant bias was indicated for the automatic and manual D dry point DP. Table 6 gives a summary of the relative bias observed for the samples used in the study.
The observed bias if any are only for the samples studied and may not be necessarily applicable to other samples. 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 method. If an agreement on which method to designate cannot be made, the referee test method will be the manual method.
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