1、Designation: E2313 08E2313 15Standard Test Method forAldehydes in Mono-, Di-, and Triethylene Glycol(Spectrophotometric Method)(using Spectrophotometry)1This standard is issued under the fixed designation E2313; the number immediately following the designation indicates the year oforiginal adoption
2、or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This test method describes the spectrophotometric determination of total ald
3、ehyde carbonyl content in the range of 0.5 to50 mg/kg (as acetaldehyde) or 0.3 to 35 mg/kg (as formaldehyde) in mono-, di-, and triethylene glycol (MEG, DEG and TEG).Alkoxyalcohols (hemiacetals), if present, are co-determined, whereas dialkoxyalkanes (acetals), if present, are not. The resultsprovid
4、e a measure of the purity of the sample with respect to total aldehyde carbonyl content.1.2 Review the current Safety Data Sheets (SDS) for detailed information concerning toxicity, first aid procedures, and safetyprecautions for all materials used in this test method.1.3 The values stated in SI uni
5、ts are to be regarded as standard. No other units of measurement are included in this standard.1.3 Review the current material Safety Data Sheets (MSDS) for detailed information concerning toxicity, first aid proceduresand safety precautions.1.4 This standard does not purport to address all of the s
6、afety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent
7、WaterD2194 Test Method for Concentration of Formaldehyde SolutionsD6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-ment System PerformanceE180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of In
8、dustrial and Specialty Chemicals(Withdrawn 2009)3E275 Practice for Describing and Measuring Performance of Ultraviolet and Visible SpectrophotometersE288 Specification for Laboratory Glass Volumetric FlasksE300 Practice for Sampling Industrial ChemicalsE969 Specification for Glass Volumetric (Transf
9、er) Pipets2.2 Other Document:Manufacturers Instruction Manual of Spectrophotometer3. Summary of Test Method3.1 The total aldehyde carbonyl content of the sample is determined spectrophotometrically. The aldehydes present are reactedwith excess 3-methyl-2-benzothiazolinone hydrazone (MBTH) to form az
10、ines.An aqueous solution of iron (III) chloride is added,causing the oxidation of the excess MBTH to a reactive cation, which reacts with the previously formed azines producingbluish-green cations. Acetone or methanol is added to stop the oxidation reaction, to mask the excess MBTH and to obtain a c
11、learsolution. The absorbance of the test solution is measured spectrophotometrically at 635 nm. The amount of aldehyde present in1 This test method is under the jurisdiction of ASTM Committee E15 on Industrial and Specialty Chemicals and is the direct responsibility of Subcommittee E15.02 onProduct
12、Standards.Current edition approved April 1, 2008Nov. 1, 2015. Published May 2008January 2016. Originally approved in 2003. Last previous edition approved in 20042008 asE2313 04.E2313 08. DOI: 10.1520/E2313-08.10.1520/E2313-15.2 For referencedASTM standards, visit theASTM website, www.astm.org, or co
13、ntactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 The last approved version of this historical standard is referenced on www.astm.org.This document is not an ASTM standard and is inte
14、nded only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the curre
15、nt versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1the test solution is derived fro
16、m a previously prepared calibration graph. The aldehyde content of the sample, expressed as eitheracetaldehyde or formaldehyde, is calculated from the data obtained.4. Significance and Use4.1 Knowledge of the total aldehyde content of Monoethylenemonoethylene glycol is required to establish whether
17、the productmeets the requirements of its quality specifications.5. Apparatus5.1 Spectrophotometer, suitable for measurement at a wavelength of 635 nm, provided with cells with a pathlength of 10mm.10 mm.NOTE 1Further information on spectrophotometers can be obtained from Practice E275.5.2 Analytical
18、 Balance, readable to 0.1 mg, calibrated. Calibrate andRecalibrate or verify at regular intervals.5.3 Stopwatch, measuring accuracy 61 s or better. Calibrate or verify Verify at regular intervals.5.4 Apparatus, as described in Test Method D2194.5.4.1 Buret, calibrated, 100-mL, 100 mL, with a 5050- o
19、r 75-mL reservoir on top of a lower portion calibrated in 0.1-mLdivisions. A PTFE-fluorocarbon resin stopcock is suitable for this purpose. Recalibrate or verify at regular intervals.5.4.2 Erlenmeyer Flask, approximately 5-mL capacity.5.4.3 Vials, specimen, short, style, approximately 5-mL capacity.
20、5.4.4 Adjustable Volume Dispensing Pipette(s), capable of dispensing volumes in the range 1.00 to 5.00 mL, with suitabledisposable pipette tips. It is recommended to verify the capacity of the pipette(s) at regular intervals.5.5 Glassware:NOTE 2In cases where volumetric glassware is to be used, it s
21、hall conform to Grade (or Class) A specifications as described in, for example,Specification E288 for volumetric flasks, or Specification E969 for one-mark pipettes.5.5.1 Graduated Pipettes, capable of quantitatively transferring between 0.5 and 5 mL, or5.5.2 Volumetric Pipette,Pipettes, 0.5, 1.0, 2
22、.0, 3.0, 4.0, 5.0 mL.mL (if no adjustable volume dispensing pipettes are used).5.5.3 Volumetric Pipettes,Pipette, 25 mL.5.5.4 Volumetric Flasks, 100 mL, 1 L.5.5.5 Brown Bottle, 1 L, with screw cap, for storage.6. Reagents6.1 Purity of ReagentsUnless otherwise indicated, it is intended that all reage
23、nts shall conform to the specifications of thecommittee on Analytical Reagents of the American Chemical Society where such specifications are available.4 Other grades maybe used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the
24、accuracyof the determination.6.1.1 Acetone (2-propanone), A.R. minimum purity 99.99 % (V/V). (WarningAcetone is highly flammable. Keep containerin a well-ventilated place. Keep away from sources of ignition. Do not breathe vapor. Take precautionary measures against staticdischarges.Warning) Acetone
25、is highly flammable. Keep container in a well-ventilated place. Keep away from sources ofignition. Do not breathe vapor. Take precautionary measures against static discharges).6.1.2 Formaldehyde, A.R., 36 to 40 % mass formaldehyde solution (Formalin). (WarningFormaldehyde is toxic byinhalation, in c
26、ontact with skin and if swallowed. Causes burns. Possible risks of irreversible effects. May cause sensitization byskin contact. In case of contact with eyes, rinse immediately with plenty of water and seek medical advice. Wear suitable protectiveclothing, gloves and eye/face protection. In case of
27、accident or if you feel unwell, seek medical advice immediately. Use only inwell ventilated areas.Warning)Formaldehyde is toxic by inhalation, in contact with skin and if swallowed. Causes burns.Possible risks of irreversible effects. May cause sensitization by skin contact. In case of contact with
28、eyes, rinse immediately withplenty of water and seek medical advice. Wear suitable protective clothing, gloves and eye/face protection. In case of accident orif you feel unwell, seek medical advice immediately. Use only in well ventilated areas.)6.1.3 Hydrochloric Acid, A.R., concentrated 36 % mass.
29、 (WarningHydrochloric Acid is toxic by inhalation. Causes severeburns. Keep container in a well-ventilated place. In case of contact with eyes, rinse immediately with plenty of water and seekmedical advice. Wear suitable protective clothing, gloves and eye/face protection. In case of accident or if
30、you feel unwell, seekmedical advice immediately.Warning)Hydrochloric Acid is toxic by inhalation. Causes severe burns. Keep container in awell-ventilated place. In case of contact with eyes, rinse immediately with plenty of water and seek medical advice. Wear suitableprotective clothing, gloves and
31、eye/face protection. In case of accident or if you feel unwell, seek medical advice immediately.)4 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For Suggestions on the testing of reagents not listed bythe American Chemical Society, see Annual
32、 Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC),(USP), Rockville, MD.E2313 1526.1.4 Iron (lll) Chloride, (FeCl36H2O), A.R. (WarningIron (III) Chloride causes burns. Avoid contact
33、with skin and eyes.In case of contact with eyes, rinse immediately with plenty of water and seek medical advice. Take off immediately allcontaminated clothing. Wear eye/face protection. If swallowed, seek medical advice immediately and show the container orlabel.Warning)Iron (III) Chloride causes bu
34、rns.Avoid contact with skin and eyes. In case of contact with eyes, rinse immediatelywith plenty of water and seek medical advice. Take off immediately all contaminated clothing. Wear eye/face protection. Ifswallowed, seek medical advice immediately and show the container or label.)6.1.5 Methanol, A
35、.R. minimum purity 99.99 % (V/V). (WarningMethanol is highly flammable. Toxic by inhalation andingestion. Keep container in a well-ventilated place. Keep container tightly closed when not in use. Keep away from sources ofignition.Avoid contact with skin. In case of accident or if you feel unwell, se
36、ek medical advice immediately (show the label wherepossible.Warning)Methanol is highly flammable. Toxic by inhalation and ingestion. Keep container in a well-ventilated place.Keep container tightly closed. Keep away from sources of ignition. Avoid contact with skin. In case of accident or if you fee
37、lunwell, seek medical advice immediately (show the label where possible).6.1.6 3-Methyl-2-Benzothiazolinone Hydrazone Hydrochloride (MBTH). (WarningMBTH is toxic if swallowed. Irritating toeyes. Keep locked up. Avoid contact with skin and eyes. In case of contact with eyes, rinse immediately with pl
38、enty of water andseek medical advice. This material and its container must be disposed of in a safe way. Wear suitable protective clothing. In caseof accident or if you feel unwell, seek medical advice immediately. If swallowed, seek medical advice immediately and show thecontainer or label.Warning)
39、MBTH is toxic if swallowed. Irritating to eyes. Keep locked up. Avoid contact with skin and eyes.In case of contact with eyes, rinse immediately with plenty of water and seek medical advice. This material and its container mustbe disposed of in a safe way. Wear suitable protective clothing. In case
40、of accident or if you feel unwell, seek medical adviceimmediately. If swallowed, seek medical advice immediately and show the container or label.)6.2 Water, reagent water conforming to Type IV of Specification D1193.6.3 Solutions:6.3.1 Standard Formaldehyde Solution, 8.0 g/mL, aqueous. Determine the
41、 exact concentration (c1) of anA.R. 36 to 40 % massformaldehyde solution (WarningSee 6.1.2WarningSee 6.1.2) according to Test Method D2194, expressing the result in g/100mL. Weigh approximately 2.0 to 2.2 g (m1) of the formaldehyde solution to the nearest 0.1 mg, into a 100-mL volumetric flask.Make
42、up to the mark with water and mix thoroughly. Pipette 1.0 mL of this solution into a 1-L volumetric flask. Make up to themark with water and mix thoroughly. Transfer this solution to a brown bottle with screw cap. Calculate the exact formaldehydecontent of this solution (c2), in g/mL, by means of th
43、e following equation:c2, g/mL5m13c110 (1)where:c1 = concentration of concentrated formaldehyde solution used, g/100 mL, andm1 = mass of concentrated formaldehyde solution taken, g.The concentrated and diluted formaldehyde solutions are stable in excess of six months if stored at room temperature. Do
44、 notstore in a refrigerator. Prepare fresh solutions every six months.6.3.2 Hydrochloric Acid, 50 %(VV). Dilute one volume of A.R. concentrated hydrochloric acid (WarningSee 6.1.3) withone volume of water.WarningSee 6.1.3) with one volume of water.6.3.3 Iron (III) Chloride Solution, 0.3 % mass, aque
45、ous. Dissolve 5 g of A.R. iron (III) chloride. 6H2O (WarningSee 6.1.4)in water, adding 1 or 2 drops of A.R. concentrated hydrochloric acid to stabilize solution (WarningSee 6.1.3WarningSee6.1.3) and dilute to 1 L with water. Prepare a fresh solution dailydaily.6.3.4 Methyl-2-benzothiazolone Hydrazon
46、e Solution (MBTH solution),0.4 % mass, aqueous. Dissolve 400 6 1 mg of MBTHhydrochloride (WarningSee 6.1.6WarningSee 6.1.6) in water in a 100-mL volumetric flask. Make up to the mark and mixthoroughly. Prepare a fresh solution daily.6.4 Reagents, as described in Test Method D2194, for the standardiz
47、ation of formaldhydeformaldehyde solution (see 6.3.1).6.4.1 Sodium Sulfite Solution, 12.5 % mass, aqueous. Dissolve 125 g of anhydrous sodium sulfite (Na2SO3) in water and diluteto 1 L.NOTE 3Sodium sulfite gradually oxidizes to sodium sulfate on exposure to air and therefore should be kept in a tigh
48、tly closed container. For bestresults freshly prepared reagent should be used.6.4.2 Sulfuric Acid, 0.5 mol/mmol/L3 (1.0 N). Prepare and standardize sulfuric acid (H2SO4) against 0.5 mol/mmol/L3 (0.5 N)sodium hydroxide (NaOH) solution which has been standardized against potassium acid phthalate to a
49、thymolphthalein end point.6.4.3 Thymolphthalein Indicator, 0.1 % mass, alcohol solution. Dissolve 1.0 g of thymolphthalein in 100 mL of methanol,ethanol, or isopropanol and dilute to 1 L with additional alcohol.6.5 Ethylene Glycol Quality Control SampleFiber It is recommended to select an Ethylene Glycol sample (fiber grade MEG,DEG or TEG (only required if maintaining a control chart, seeTEG), similar to the product being analyzed and to use it as a qualitycontrol sample (WarningSee 7.2). 10.9). Store at a temperature between 0 and 5C. Warm to
