1、Designation: D4337 89 (Reapproved 2009)Standard Test Methods forAnalysis of Linear Detergent Alkylates1This standard is issued under the fixed designation D4337; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revi
2、sion. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 These test methods cover chemical and physical testsapplicable to linear detergent alkylates, evaluating those prop-erties whic
3、h characterize linear detergent alkylates with respectto its suitability for desired uses.NOTE 1Linear detergent alkylates comprises linear alkylbenzenesprepared by varying processes of varying linear alkyl chain length. Thealkylate is sulfonated for surfactant use, the largest application being ind
4、etergent products. Careful control of linear detergent alkylate character-istics is desired; during sulfonation, variations of the sulfonate can occurthat may result in either desirable or undesirable end-use properties.1.2 The test methods appear as follows:SectionComposition by Gas Chromatography
5、7-15Chlorides 16-27Color 28-30Refractive Index 31-33Specific Gravity 34-36Water 37-391.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices an
6、d determine the applica-bility of regulatory limitations prior to use. Material SafetyData Sheets are available for reagents and materials. Reviewthem for hazards prior to usage. See also Note 1 and Section21.2. Referenced Documents2.1 ASTM Standards:2D270 Methods of Sampling Petroleum and Petroleum
7、 Prod-ucts3D1122 Test Method for Density or Relative Density ofEngine Coolant Concentrates and Engine Coolants By TheHydrometerD1193 Specification for Reagent WaterD1209 Test Method for Color of Clear Liquids (Platinum-Cobalt Scale)D1218 Test Method for Refractive Index and RefractiveDispersion of H
8、ydrocarbon LiquidsD1364 Test Method for Water in Volatile Solvents (KarlFischer Reagent Titration Method)E180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals33. Significance and Use3.1 These test methods are suitable for setting s
9、pecificationson linear detergent alkylates and for quality control wherethese alkylates are manufactured or are used in a manufactur-ing process.3.2 The gas chromatography test is useful in identifyinglinear detergent alkylates produced by the various manufactur-ing processes and for determining the
10、 applicability of a lineardetergent alkylate to a particular end use. Test conditions havebeen optimized for resolution of the C-9 to C-15 lineardetergent alkylates and the presence of higher or lower chainlengths will be readily apparent but may produce erroneousresults. The tetralin structures hav
11、e not been sufficientlyidentified to allow determination of tetralins, and small uni-dentified components are reported as tetralins and unidenti-fieds.3.3 Some linear detergent alkylates use a manufacturingprocess with an organic chloride as a precursor. This test maybe used to ensure that the chlor
12、ide content of the alkylate is notexcessive for a particular end use.3.4 The platinum-cobalt color test is useful in determiningthat the color of the linear detergent alkylate will not contributeto the color of the end use product.3.5 The refractive index and specific gravity tests arepossible aids
13、in the identification of linear detergent alkylatesand in evaluating alkylates for gross contaminants.1These test methods are under the jurisdiction of ASTM Committee D12 onSoaps and Other Detergents and are the direct responsibility of SubcommitteeD12.12 on Analysis and Specifications of Soaps, Syn
14、thetics, Detergents and theirComponents.Current edition approved Oct. 1, 2009. Published March 2010. Originallyapproved in 1984. Last previous edition approved in 2003 as D4337 89(2003).DOI: 10.1520/D4337-89R09.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Cust
15、omer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn. The last approved version of this historical standard is referencedon www.astm.org.1Copyright ASTM International, 100 Barr Harbor Drive, P
16、O Box C700, West Conshohocken, PA 19428-2959, United States.3.6 The water test is suitable for determining that lineardetergent alkylates do not contain amounts of water deleteriousto further processing.4. Purity of Reagents4.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unl
17、ess otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee onAnalytical Reagents of theAmerican Chemical Society,4where such specifications are available. Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently
18、high purity to permit its use without lessening theaccuracy of the determination.4.2 Unless otherwise indicated, references to water shall beunderstood to mean Type III water conforming to SpecificationD1193.5. Precautions5.1 Consult the latest OSHA regulations regarding all re-agents and materials
19、used in these test methods.56. Sampling6.1 Unless otherwise indicated in a specific test method,sample the material in accordance with Method D270, withspecial application of Sections 41 and 42 pertaining to indus-trial aromatic hydrocarbons, Section 12 pertaining to Bottle orBeaker Sampling, and Se
20、ction 15 pertaining to Tap Sampling.Samples must be taken and stored in amber, screw-cap, glassbottles to protect them from light.COMPOSITION BY GAS CHROMATOGRAPHY7. Scope7.1 The gas chromatography test was developed to allowdetermination of C-9 through C-15 linear detergent alkylateisomer distribut
21、ion before sulfonation. The analyses of stockshaving a chain length distribution above or below the intervalcovered in this test method will require a different set ofoperating conditions. If water, extremely high boiling compo-nents, or unusual impurities are present in the linear detergentalkylate
22、, this test would not necessarily detect them and mayproduce erroneous results.8. Summary of Test Method8.1 A sample is injected by means of a microsyringe into avaporization chamber of a gas chromatograph.Astream splitterallows the majority of the sample to be vented into theatmosphere through a va
23、lve that is incorporated in the vapor-ization chamber.Asmall portion of the sample is then swept bythe carrier gas into a capillary column that has been coated witha thin layer of the stationary phase. A hydrogen flame ioniza-tion detector provides a very sensitive means of detecting theextremely sm
24、all concentrations of separated vapor componentsas they elute from the column. An electrometer-amplifierconverts the detector signal into a suitable signal that can berecorded on a standard strip-chart recorder and integrated by asuitable integration device. The concentrations of the compo-nents are
25、 obtained by normalizing the integrated areas, basedon the assumption that all components of the mixture are elutedunder the conditions used.9. Apparatus9.1 Gas Chromatograph, with the following characteristics:9.1.1 Sample Injection Port, operable at 250C and contain-ing a stream splitter capable o
26、f linearly splitting sampleinjections up to 1000 to 1.9.1.2 Column Oven, capable of temperature programmingfrom 120 to 165C at a rate of 1 or 2C per min.9.1.3 Flame Ionization Detector, capable of operating at300C.9.2 Recorder, 0 to 1 mv range with 0.1 second full scaledeflection.9.3 Integration Dev
27、ice, capable of accurately measuringareas of up to 250 components.9.4 Column, 150 ft (45.7 m) by 0.01 in. (0.25 mm) insidediameter stainless steel wall; open tubular capillary column4Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestio
28、ns on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.5Available from Occupational Safet
29、y and Health Review Commission, 1825 KStreet, Washington, DC 20006.FIG. 1 Typical Gas Chromatic Scan of an AlkylateD4337 89 (2009)2coated with phenyl methyl silicone DC-5506or other columnthat will perform required separation as indicated in Fig. 1.9.5 Syringe, 10-L capacity with fixed 2-in. (5.1 cm
30、)needle.710. Reagents10.1 Carrier Gas, high-purity nitrogen.10.2 Hydrogen, 99.996 mol % pure.10.3 Compressed Air.11. Calibration11.1 No calibration or correction factors are necessary as theresponse of the flame ionization detector is essentially constantfor aromatic hydrocarbons. The individual pea
31、k area percent-ages may be regarded as the actual weight percent in thesample.12. Procedure12.1 Adjust the chromatograph to the following conditions:Column temperature, C (Note 2) 120 programmed to 160 at 1 to 2Cper minInjection port temperature, C 250Detector temperature, C 300Carrier gas pressure,
32、 lbf 60Sample size (Note 3), L 0.5 to 1Chart speed, cm/min 1Hydrogen flow (Note 4), mL/min 30Air flow (Note 4), mL/min 240Range X1Attenuator setting X4Splitter (Note 3) 1000/1NOTE 2These conditions should give adequate separation. It may benecessary to adjust conditions slightly to meet the separati
33、on criteria of thesample chromatogram (Fig. 1), depending upon the performance of thecapillary column.NOTE 3Sample size and splitter ratio should be adjusted to obtain apeak height of 10 to 15 mV for the largest components.NOTE 4Hydrogen and air flows should be adjusted to give maximumdetector sensi
34、tivity. See instructions in instrument instruction manual.12.2 When a new column is installed, leak-test the plumb-ing connections by applying the operating carrier gas pressure.The air and hydrogen connections to the detector should beleak tested periodically. In particular, the hydrogen supplyshou
35、ld be leak-tested at the cylinder each time the cylinder ischanged, due to the hazardous nature of hydrogen gas.12.3 Wet and rinse the syringe with the sample and draw anexcess of liquid into the syringe barrel. Exercise caution that allair bubbles are excluded from the liquid in the syringe.Careful
36、ly depress the plunger until the exact amount of liquiddesired is contained in the syringe.12.4 Open the split valve and quickly pierce the septum,thrusting the needle of the syringe completely into the inlet. Inthe same motion quickly and completely depress the plunger.Immediately withdraw the syri
37、nge and start the column oventemperature program sequence. The split valve may be closed1 min after the injection of the sample, but it must always beclosed at exactly the same time after injection.12.5 Compare the sample chromatogram with the standardchromatogram (Fig. 1) and from the retention tim
38、es of thecomponents identify all straight chain alkyl benzene isomers.Label all peaks whose identity has been established. Manyunidentified minor peaks will appear as minor constituents ofthe sample and may be attributed to tetralin structures. Includethese peaks in the calculations and report in a
39、pooled percent-age as tetralins and unknowns.13. Calculations13.1 Calculate the percentage for each component by divid-ing the area of each component by the total area of allcomponents and multiplying by 100.13.2 Calculate the total 2-phenyl isomer by summing to-gether the 2-phenyl isomers for all c
40、hain lengths.13.3 Calculate the chain length distribution by summingtogether all percentages for the identified linear alkyl benzeneisomers of each chain length.13.4 Calculate lights (components eluting before C10alkylbenzene) by summing together the percentages of all thecomponents eluting before 5
41、-phenyldecane.13.5 Calculate heavies (components eluting after C14alkylbenzene) by summing together all the percentages of thecomponents eluting after 2-phenyltetradecane.13.6 Calculate tetralins and unknowns by summing togetherthe percentages of all unidentified peaks eluting between the5-phenyldec
42、ane peak and the 2-phenyltetradecane peak.13.7 Determine the average molecular weight by assumingthe tetralins and unknowns to have a molecular weight of 244.The average molecular weight is calculated to the third decimalplace using the following equation:Average molecular weight 5 100 2lights (1)1
43、heavies!#/( C10isomers/218!1 ( C11isomers/232! 1 ( C12isomers/246!1 ( C13isomers/260! 1 ( C14isomers/274!1 ( tetralins 1 unknowns/244!#14. Report14.1 Report the components and average molecular weightas specified in Table 1. Duplicate runs that agree within thechecking limits shown in Table 1 are ac
44、ceptable for averaging(95 % confidence level).15. Precision and Bias15.1 The following criteria should be used for judging theacceptability of results:15.1.1 Repeatability (Single Analyst) The standard devia-tion of results (each the average of duplicates), obtained by thesame analyst on different d
45、ays, has been estimated to be thevalue shown in Table 1 with the indicated degrees of freedom.Two such results should be considered suspect (95 % confi-dence level) if they differ by more than the values in Table 1.15.1.2 Reproducibility (Multilaboratory) The standarddeviation of results (each the a
46、verage of duplicates), obtainedby analysts in different laboratories, has been estimated to bethe value shown in Table 1 with the indicated degrees of6Capillary column, Part 009-0354, available from Perkin-Elmer Corporation,Norwalk, CT, has been found satisfactory.7Microsyringe No. 701, available fr
47、om Hamilton Co., P. O. Box 307, Whittier,CA, has been found satisfactory.D4337 89 (2009)3freedom. Two such results should be considered suspect (95 %confidence level) if they differ by more than the values shownin Table 1 (Note 5).NOTE 5The preceding precision estimates are based on an interlabo-rat
48、ory study of six samples of linear detergent alkylates. A total of eightlaboratories cooperated in the studies in which duplicate determinationswere performed on each of 2 days. Practice E180 was used in developingthese precision estimates.ORGANIC CHLORIDES16. Scope16.1 This test method is suitable
49、for the rapid determinationof organic chlorides in linear detergent alkylates before sul-fonation. The test method is applicable to samples whichinclude chloride-containing compounds that are volatile at700C. Compounds such as sodium chloride do not completelyvolatilize under the operating conditions specified and are notquantified. By using the proper sample size, this test method isapplicable to the direct detection of chlorides at levels up to700 ppm. Halogen compounds other than those containingchlorides tend to be nonquantitatively detected by this
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