欢迎来到麦多课文档分享! | 帮助中心 海量文档,免费浏览,给你所需,享你所想!
麦多课文档分享
全部分类
  • 标准规范>
  • 教学课件>
  • 考试资料>
  • 办公文档>
  • 学术论文>
  • 行业资料>
  • 易语言源码>
  • ImageVerifierCode 换一换
    首页 麦多课文档分享 > 资源分类 > PDF文档下载
    分享到微信 分享到微博 分享到QQ空间

    ASTM E2403-2006(2012) Standard Test Method for Sulfated Ash of Organic Materials by Thermogravimetry《用热解重量分析法测定有机材料的硫酸盐灰分的标准试验方法》.pdf

    • 资源ID:531060       资源大小:70.33KB        全文页数:3页
    • 资源格式: PDF        下载积分:5000积分
    快捷下载 游客一键下载
    账号登录下载
    微信登录下载
    二维码
    微信扫一扫登录
    下载资源需要5000积分(如需开发票,请勿充值!)
    邮箱/手机:
    温馨提示:
    如需开发票,请勿充值!快捷下载时,用户名和密码都是您填写的邮箱或者手机号,方便查询和重复下载(系统自动生成)。
    如需开发票,请勿充值!如填写123,账号就是123,密码也是123。
    支付方式: 支付宝扫码支付    微信扫码支付   
    验证码:   换一换

    加入VIP,交流精品资源
     
    账号:
    密码:
    验证码:   换一换
      忘记密码?
        
    友情提示
    2、PDF文件下载后,可能会被浏览器默认打开,此种情况可以点击浏览器菜单,保存网页到桌面,就可以正常下载了。
    3、本站不支持迅雷下载,请使用电脑自带的IE浏览器,或者360浏览器、谷歌浏览器下载即可。
    4、本站资源下载后的文档和图纸-无水印,预览文档经过压缩,下载后原文更清晰。
    5、试题试卷类文档,如果标题没有明确说明有答案则都视为没有答案,请知晓。

    ASTM E2403-2006(2012) Standard Test Method for Sulfated Ash of Organic Materials by Thermogravimetry《用热解重量分析法测定有机材料的硫酸盐灰分的标准试验方法》.pdf

    1、Designation: E2403 06 (Reapproved 2012)Standard Test Method forSulfated Ash of Organic Materials by Thermogravimetry1This standard is issued under the fixed designation E2403; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the yea

    2、r 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. Scope1.1 This standard describes the determination of sulfatedash content (sometimes called residue-on-ignition) of organi

    3、cmaterials by thermogravimetry. The method converts commonmetals found in organic materials (such as sodium, potassium,lithium, calcium, magnesium, zinc, and tin) into their sulfatesalts permitting estimation of their total content as sulfates oroxides. The range of the test method is from 0.1 to 10

    4、0 %metal content.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 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

    5、to establish appro-priate safety and health practices and to determine theapplicability of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D874 Test Method for Sulfated Ash from Lubricating Oilsand AdditivesD914 Test Methods for EthylcelluloseD3516 Test Methods for Ash

    6、ing CelluloseE473 Terminology Relating to Thermal Analysis and Rhe-ologyE1131 Test Method for Compositional Analysis by Thermo-gravimetryE1142 Terminology Relating to Thermophysical PropertiesE1582 Practice for Calibration of Temperature Scale forThermogravimetryE2040 Test Method for Mass Scale Cali

    7、bration of Thermo-gravimetric Analyzers2.2 Other Standards:The United States Pharmacopeia XXII and The NationalFormulary XVII, United States PharmacopeialConvention, Rockville, MD, 1990, Section 281, p. 15273. Terminology3.1 DefinitionsTechnical terms used in this standard aredefined in Terminologie

    8、s E473 and E1142.3.1.1 sulfated ash, nthe residue remaining after a speci-men has been oxidized, and the residue subsequently treatedwith sulfuric acid and heated to constant weight.3.1.2 residue-on-ignition, ROI, na commonly used aliasfor sulfated ash.3.1.3 volatiles, nfor the purpose of this test,

    9、 those mate-rials evolving as gas at temperatures below 160C in an airatmosphere.4. Summary of Test Method4.1 A test specimen is ignited and burned in an air atmo-sphere at temperatures up to 600C until only ash remains.After cooling, the residue is treated with sulfuric acid andheated to 800C to co

    10、nstant weight. The residue remaining isidentified as sulfated ash.4.2 This test method is similar to Test Method D874 forlubricating oils and additives, Test Methods D914 for ethylcellulose, Test Methods D3516 cellulose, and that of TheUnited States Pharmacopeia XXII and makes use of thermo-gravimet

    11、ric apparatus to perform the determination.5. Significance and Use5.1 The sulfated ash may be used to indicate the level ofknown metal-containing additives or impurities in an organicmaterial. When phosphorus is absent, barium, calcium,magnesium, sodium and potassium are converted to theirsulfates.

    12、Tin and zinc are converted to their oxides.5.2 This standard may be used for research anddevelopment, specification acceptance and quality assurancepurposes.6. Interferences6.1 If phosphorus is present with metals, it partially orwholly remains in the sulfated ash as metal phosphates.1This test meth

    13、od is under the jurisdiction ofASTM Committee E37 on ThermalMeasurements and is the direct responsibility of Subcommittee E37.01 on Calo-rimetry and Mass Loss.Current edition approved Sept. 1, 2012. Published September 2012. Originallyapproved in 2004. Last previous edition approved in 2006 as E2403

    14、 06. DOI:10.1520/E2403-06R12.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 10

    15、0 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States16.2 Sulfur and chlorides do not interfere.7. Apparatus7.1 Thermogravimetric Analyzer (TGA)The essential in-strumentation required to provide the minimum thermogravi-metric analytical capability for this standard includ

    16、es:7.1.1 A thermobalance composed of:7.1.1.1 A furnace to provide uniform controlled heating of aspecimen to a constant temperature of 850C and at a constantrate of 5 to 60C/min7.1.1.2 A temperature sensor to provide an indication of thespecimen or furnace temperature to 61C.7.1.1.3 A continuously r

    17、ecording balance to measure thespecimen mass with a minimum capacity of 50 mg and asensitivity of 60.01 mg.7.1.1.4 A means of maintaining the specimen or containerunder atmospheric control of air at a purge flow rate of 50 to100 mL/min 6 5 mL/min.7.1.2 A temperature controller capable of executing a

    18、 spe-cific temperature program by operating the furnace betweenselected temperature limit at a rate of 5 to 60C/min and to anisothermal temperature of up to 850C which is maintainedconstant to 610C for a minimum of 70 minutes.7.1.3 A recording device, capable of recording and display-ing any fractio

    19、n of the specimen mass signal (TGA curve)including signal noise.7.1.4 Containers (pans, crucibles, etc.) that are inert to thespecimen and to concentrated sulfuric acid and that will remaingravimetrically stable up to 850C. Platinum is a commonmaterial of construction for this purpose.7.2 Graduated

    20、micropipette with capacity of 4050 L8. Reagents and Materials8.1 Sulfuric acid, concentrated (98 %), with a relativedensity of 1.84. (WarningPoison. Corrosive. Strong Oxi-dizer.)8.2 AirZero grade or better purity9. Hazards9.1 Sulfuric acid may be corrosive to some thermogravimet-ric apparatus. A reg

    21、ular visual inspection of the apparatus willdetermine if any corrosion is taking place.9.2 The exhausted purge gas from the apparatus will containsulfuric acid fumes. This purge gas shall be treated byexhausting to a acid hood or by bubbling through a solution ofsodium bicarbonate to absorb the acid

    22、ic fumes.10. Preparation of Apparatus10.1 After turning the power on, allow the instrument toequilibrate for at least one hour prior to any measurements.10.2 Perform any cleaning and calibration procedures de-scribed by the manufacturer in the apparatus OperatorsManual.11. Calibration and Standardiz

    23、ation11.1 Perform temperature calibration of the thermogravi-metric analyzer according to Practice E1582 using referencematerials suitable for the temperature range of this method,namely 25 to 800C.11.2 Perform mass calibration of the thermogravimetricanalyzer according to Test Method E2040.12. Proc

    24、edure12.1 Transfer 30 to 40 mg of the sample into a tared, clean,and dry sample container. Assemble the thermogravimetricanalyzer for operation. Record the initial weight of the testspecimen as Woto within 60.01 mgNOTE 1The sample container may be preconditioned by heating in anair atmosphere to 800

    25、C.NOTE 2Smaller quantities of test specimen will reduce the quantifi-cation capability of this method.12.2 Heat the specimen from ambient to 600C at 10C/minunder an air purge gas with a flow rate of 50 to 100 6 5mL/min and record the thermal curve.12.3 Cool the heated sample and thermogravimetric ap

    26、pa-ratus to 20 to 25C.12.4 If desired, record the weight at 150C (Wv) as the massafter apparent loss of volatiles. Record the weight at 600C asthe mass of the residue (Wr).NOTE 3Mass loss due to apparent loss of volatiles at 150C andresidue at 600C are not required for the sulfated ash determination

    27、 butmay be recorded for additional sample characterization (see Test MethodE1131.)NOTE 4The temperature at which the mass loss due to volatiles isdetermined may range from 100 to 160C depending upon the material.Other values may be used but shall be reported.12.5 Using a micropipette, add 30 40 L of

    28、 98 % gradesulfuric acid to the sample residue (in the container). Reas-semble the instrument for operation.12.6 Heat the specimen from ambient to 800C at 50C/minand hold isothermally at 800 6 25C for 60 6 1 minutes underan air purge at 50 to 100 6 5 mL/min.12.7 Cool the heated specimen and thermogr

    29、avimetric ap-paratus to 20 to 25C.12.8 Record the residue mass Ws.12.9 Calculate percent Sulfated Ash (S) using Eq 1.12.10 In the absence of interferences and if the specificmetal in the test specimen is known, then its mass percent (M)may be calculated by multiplying the sulfated ash value by thefa

    30、ctors presented in Table 1 using Eq 2.TABLE 1 Sulfated Ash FactorsMetal Sulfated Ash FactorSodium (Na) Na2SO40.3237Potassium (K) K2SO40.4487Lithium (Li) Li2SO40.1263Calcium (Ca) CaSO40.2944Magnesium (Mg) MgSO40.2019Zinc (Zn) ZnO 0.8034Tin (Sn) SnO 0.8812E2403 06 (2012)212.11 If desired, calculate th

    31、e Percent Volatiles (V) andPercent Residue (R) using equations 3 and 4, respectively.13. Calculation13.1 Sulfated Ash (S) may be determined using the follow-ing equation:S 5 Ws3100 %/Wo(1)where:S = Sulfated ash, mass %,Ws= Mass of sulfated ash from Section 12.8, mg,Wo= Original mass of the test spec

    32、imen from Section 12.1,mg.13.2 If the specific metal in the test specimen is known andif this is the only metal ion present, then its mass percent (M)may be calculated by multiplying the sulfated ash value by thefactors presented in Table 1 using Eq 2.M metal! 5 Factor 3 S (2)where:M = Percent of th

    33、e identified metal, mass %.14. Report14.1 Report the sulfated ash (S) to three significant figures.14.2 Report to three significant figures the percent metal(M) when desired and the metal is known.14.3 Provide a copy of the original thermal curve.14.4 The specific dated version of this test method u

    34、sed.15. Precision and Bias15.1 An interlaboratory study was conducted in 2005 inwhich lithium cyclohexanebutyrate and calcium oxalate mono-hydrate were tested. Eight laboratories participated in the testusing seven instrument models from two manufacturers. AResearch Report is available from ASTM Hea

    35、dquarters.315.2 Precision:15.2.1 Within laboratory variability may be described usingthe repeatability value (r) obtained by multiplying the repeat-ability standard deviation by 2.8. The repeatability valueestimates the 95 % confidence limit. That is, two results fromthe same laboratory should be co

    36、nsidered suspect (at the 95 %confidence level) if they differ by more than the repeatabilityvalue.15.2.1.1 The within laboratory repeatability standard devia-tion for lithium in lithium cyclohexanebutyrate was 0.057 %(RSD of 1.5 %) with 20 degrees of experimental freedom.15.2.1.2 The within laborato

    37、ry repeatability standard devia-tion for calcium in calcium oxalate monohydrate was 0.24 %(RSD of 0.92 %) with 20 degrees of experimental freedom.15.2.2 Between laboratory variability may be describedusing the reproducibility value (R) obtained by multiplying thereproducibility standard deviation by

    38、 2.8. The reproducibilityvalues estimates the 95 % confidence limit. That is, two resultsobtained from different laboratories, operators or apparatusshould be considered suspect (at the 95 % confidence level) ifthey differ by more than the reproducibility value.15.2.2.1 The between laboratory reprod

    39、ucibility standarddeviation for lithium in lithium cyclohexanebutyrate was 0.10% (RSD = 2.5 %) with 20 degrees of experimental freedom.15.2.2.2 The between laboratory reproducibility standarddeviation for calcium in calcium oxalate monohydrate was0.32 % (RSD = 1.2 %) with 20 degrees of experimentalf

    40、reedom.15.3 Bias:15.3.1 Bias is the difference between the mean value ob-tained and an accepted reference value for the same material.15.3.1.1 The lithium cyclohexanebutyrate used in this studywas supplied (by Sigma-Aldrich, St. Louis, MO) with aCertificate of Analysis indicate an ICP assay of 3.9 %

    41、 lithium.The sample is 3.94 % lithium by formula weight.15.3.1.2 The mean value for lithium in lithium cyclo-hexanebutyrate characterized by this method was found to be3.93 %, indicating no detectable bias in this method.16. Keywords16.1 ash; residue on ignition; sulfated ash; thermogravimet-ric ana

    42、lysis; thermogravimetryASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringem

    43、ent of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or

    44、 for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views kn

    45、own to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting AS

    46、TM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).3Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:E37-1036.E2403 06 (2012)3


    注意事项

    本文(ASTM E2403-2006(2012) Standard Test Method for Sulfated Ash of Organic Materials by Thermogravimetry《用热解重量分析法测定有机材料的硫酸盐灰分的标准试验方法》.pdf)为本站会员(inwarn120)主动上传,麦多课文档分享仅提供信息存储空间,仅对用户上传内容的表现方式做保护处理,对上载内容本身不做任何修改或编辑。 若此文所含内容侵犯了您的版权或隐私,请立即通知麦多课文档分享(点击联系客服),我们立即给予删除!




    关于我们 - 网站声明 - 网站地图 - 资源地图 - 友情链接 - 网站客服 - 联系我们

    copyright@ 2008-2019 麦多课文库(www.mydoc123.com)网站版权所有
    备案/许可证编号:苏ICP备17064731号-1 

    收起
    展开