1、Designation: D2109 01(Reapproved 2011)Standard Test Methods forNonvolatile Matter in Halogenated OrganicSolvents and Their Admixtures1This standard is issued under the fixed designation D2109; the number immediately following the designation indicates the year oforiginal adoption or, in the case of
2、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.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 These test meth
3、ods cover the determination of nonvola-tile matter in halogenated organic solvents and admixtures.1.2 Five test methods are covered, as follows:1.2.1 Test Method AFor halogenated organic solvents oradmixtures having less than 50 ppm nonvolatile matter; orwhere precision better than 610 ppm is requir
4、ed.1.2.2 Test Method BFor halogenated organic solvents oradmixtures having more than 50 ppm nonvolatile matter orwhere precision of 60.001 % (10 ppm) is satisfactory.1.2.3 Test Method CFor low-boiling halogenated organicsolvents or their admixtures (for example, methylene chloride,trichlorotrifluoro
5、ethane) that may superheat and cause bump-ing while evaporating to dryness with steam. A precision ofgreater than6 10 ppm can be attained.1.2.4 Test Method DFor rapid measurement of nonvola-tile matter in halogenated organic solvents and their admixturesand where precision better than 610 ppm is req
6、uired.1.2.5 Test Method EFor halogenated organic solvents oradmixtures and where precision better than 610 ppm isrequired.1.3 The values stated in SI units are to be regarded as thestandard.1.4 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in
7、 thisstandard.1.5 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 and determine the applica-bility of regulatory limitations prior to use.2
8、. Terminology2.1 Definitions of Terms Specific to This Standard:2.1.1 The term nonvolatile matter should not be construedas equivalent to residue on ignition, ignition residue, or ashcontent. Particulates, sediments, and suspended matter shouldnot be considered part of nonvolatile matter. If these s
9、olids arepresent in the sample, they should be removed by filtration ordecantation prior to beginning this test method. Nonvolatilematter is considered to be “in solution” with the solvent andthat which will become residual upon drying the solvent at aspecified temperature.2.1.2 Nonvolatile matter a
10、nd nonvolatile residue are inter-changeable terms.3. Significance and Use3.1 Nonvolatile matter in solvents can adversely affect theircleaning properties. These test methods can be used to controlsoil contamination in the boiling solvent, which if allowed tobecome too high, can decrease the stabilit
11、y of the solvent.3.2 These test methods can be used to establish manufac-turing and purchasing specifications.4. Apparatus4.1 Oven, thermostatically controlled at 105 6 5C.4.2 Evaporating Dish, 125-mL capacity, platinum or high-silica glass, Methods A, B, C.4.3 Evaporating Dish (80 3 45 or 115 3 50)
12、 (Method D).4.4 Steam Bath (or hot plate).4.5 Hot Plate, (Method D).4.6 Heat Lamp, 250 W, (Method E).4.7 Analytical Balance, capable of measuring to 0.0001 g.4.8 Top Loading Balance, capable of weighing to 0.01 g.4.9 Aluminum Weighing Dish,573 18 mm, (Method D).4.10 Aluminum Weighing Dish, 200 ML ca
13、pacity, (MethodE).4.11 1000-mL Volumetric Flask (Test Method A).4.12 100-mL Volumetric Pipet (Test Method B and E).4.13 1000-mL Graduated Cylinder (Test Method C).4.14 1500-mL Erlenmeyer Flask (Test Method C).1These test methods are under the jurisdiction of ASTM Committee D26 onHalogenated Organic
14、Solvents and Fire Extinguishing Agents and are the directresponsibility of Subcommittee D26.04 on Test Methods.Current edition approved Aug. 1, 2011. Published November 2011. Originallyapproved in 1962 as D2109 62 T. Last previous edition approved in 2006 asD2109 01 (2006)1. DOI: 10.1520/D2109-01R11
15、.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.TEST METHOD A5. Procedure5.1 Dry a 125-mL capacity platinum (or high-silica glass)evaporating dish in an oven at 105 6 5C and cool in adesiccator. Repeat until the weight is constant o
16、r within 0.1 mgof the last weighing. Rinse a clean dry 1000-mL volumetricflask with the solvent and fill to the 1000-mL mark with thesolvent to be tested. Invert the evaporating dish, place it overthe mouth of the flask, hold it firmly in place, and invert theflask. In this position place both dish
17、and flask on a steam bath.Adjust a ring support to hold the flask so the mouth of the flaskis approximately 25 mm above the bottom of the evaporatingdish. Thus held, the flask automatically feeds the solvent to thedish during the evaporation. (WarningThis test methodmust be run in a ventilated, dust
18、-free area.)5.2 Evaporate the 1000-mL sample to dryness. Remove thedish from the steam bath with metal tongs and blot the outsideof the dish with lint-free paper tissue.NOTE 1Hot plates develop high temperatures on the plate surface. Ifa hot plate is used to evaporate the solvent, the evaporating di
19、sh should beplaced inside a water bath while on the hot plate to prevent the samplefrom reaching temperatures exceeding 105C.5.3 Place the dish and contents in an oven at 105 6 5C forapproximately 1 h. Cool in a desiccator and weigh the dish andcontents.6. Calculation6.1 Calculate the nonvolatile ma
20、tter and report in weightpercent or parts per million as follows:Nonvolatile matter, ppm by weight 5A! 106!B! 1000!5A! 1000!B!(1)where:A = grams of residue, andB = density of sample.7. Precision and Bias7.1 Repeatability (Single Analyst)The standard deviationof results has been estimated to be 0.2 w
21、eight ppm. Two suchvalues should be considered suspect (95 % confidence level) ifthey differ by more than 0.7 ppm.7.2 Reproducibility (Multilaboratory)The standard de-viation of results has been estimated to be 1.0 weight ppm. Twosuch values should be considered suspect (95 % confidencelevel) if the
22、y differ by more than 4.6 weight ppm.TEST METHOD B8. Procedure8.1 Dry a 125-mL capacity platinum (or high-silica glass)evaporating dish in an oven at 105 6 5C and cool in adesiccator. Repeat until the weight is constant or within 0.1 mgof the last weighing. Pipet 100 mL of sample into the dish andpl
23、ace on a steam bath.8.2 Evaporate the sample to dryness as in Section 5 (seeNote 1 and Note 1). Remove the dish from the steam bath withmetal tongs and blot the outside of the dish with lint-free papertissue.8.3 Place the dish and contents in an oven at 105 6 5C forapproximately 1 h. Cool in a desic
24、cator and weigh the dish andcontents.9. Calculation9.1 Calculate the nonvolatile matter and report in weightpercent as follows:Nonvolatile matter, ppm by weight 5A! 100!B! 100!5A!B!(2)where:A = grams of residue, andB = density of sample.10. Precision and Bias10.1 PrecisionAs the only significant dif
25、ference betweenTest Method B and Test Methods A and C is the sample size(100 mL versus 1000 mL), it is reasonable to assume that theprecision is roughly ten times that of Test Methods A and C or2 ppm for repeatability and 10 ppm for reproducibility.10.2 The bias of this test method has not been dete
26、rmined.TEST METHOD C11. Procedure11.1 Dry a 125-mL capacity platinum (or high-silica glass)evaporating dish in an oven at 105C and cool in a desiccator.Repeat until the weight is constant or within 0.1 mg of the lastweighing. Rinse a clean dry 1000-mL graduated cylinder and a1500-mL Erlenmeyer flask
27、 with the solvent to be tested.11.2 Measure 1000 mL of the sample into the cleanedgraduate and transfer 970 mL of it into the clean Erlenmeyerflask. Evaporate to about 40 mL on a steam bath or warm hotplate in a fume hood. Do not evaporate to dryness.11.3 Transfer the residue to the evaporating dish
28、. Rinse theflask twice with a 15-mL portion of the sample retained in thegraduate (see Note 2). Add the rinsings to the evaporating dish.NOTE 2All of the retained sample is used to rinse the beaker and mustbe included in the sample volume.11.4 Allow the sample to evaporate by gently heating on awarm
29、 hotplate. Protect the evaporating dish from externalcontamination and do not exceed 60C (140F). When evapo-ration is complete, dry the evaporating dish in the oven at105C for 30 min, cool in a desiccator for 30 min, and reweigh.12. Calculation12.1 Calculate the nonvolatile matter and report in part
30、s permillion as follows:Nonvolatile matter, ppm by weight 5A! 106!B! 1000!5A! 1000!B!(3)where:A = grams of residue, andB = density of sample.13. Precision and Bias13.1 Repeatability (Single Analyst)The standard devia-tion of results has been estimated to be 0.2 weight ppm. TwoD2109 01 (2011)2such va
31、lues should be considered suspect (95 % confidencelevel) if they differ by more than 0.7 ppm.13.2 Reproducibility (Multilaboratory)The standard de-viation of results has been estimated to be 1.0 weight ppm. Twosuch values should be considered suspect (95 % confidencelevel) if they differ by more tha
32、n 4.6 weight ppm.TEST METHOD D14. Procedure14.1 Weigh 100 g of sample on a top loading balance into anevaporating dish (80 3 45 or 115 3 50) and place it on the hotplate. Record the sample weight. Adjust the heat so that thesample boils away without spattering or splashing out of thedish. Evaporatio
33、n of the solvent must be carried out in a fumehood.14.2 While the sample is evaporating, weigh an aluminumweighing dish to 0.0001 g and record the weight W1.14.3 Evaporate the sample to within 8 to 12 mL of drynessand transfer it to the weighed aluminum weighing dish usingmetal tongs.14.4 Place the
34、aluminum weighing dish on the hot plate andevaporate until only a small amount of liquid (about 1 mL)remains.14.5 Transfer the aluminum weighing dish to an oven set at105C and leave it for 30 min.14.6 Remove the dish from the oven, allow it to cool for 1min and weigh the dish. Record the weight as W
35、2.Itisnotnecessary to cool the dish in a dessicator.14.7 Calculate the nonvolatile matter (NVM) by the for-mula:PPM NVM 5W22 W1! X 1 000 000sample weight(4)14.8 In many cases the analysis can be done faster in thefollowing way:14.8.1 Leave the sample in the 105C oven until the dish isfree of liquid
36、but not more than 30 min.14.8.2 When the dish is free of liquid, remove it from theoven and cool it for 1 min. Weigh the dish. If the calculationshows the result to be less than one ppm, the test may bestopped and the results recorded.14.8.3 If there is measurable NVM (1 ppm) in the dish,return it t
37、o the oven for 30 min and proceed beginning with14.6.15. Precision and Bias215.1 The standard deviation of results of a single analystover different days was determined to be 1.8 ppm at a level of10 ppm nonvolatile matter.15.2 The standard deviation of results from multiple labo-ratories over multip
38、le days was determined to be 2.2 ppm at alevel of 10 ppm nonvolatile matter.15.3 Overall recovery for this method was 104.5 % fromapproximately 1 ppm to approximately 1000 ppm nonvolatilematter.15.4 The low quantification limit is approximately 1 ppm.TEST METHOD E16. Procedure16.1 Dry a 200 mL capac
39、ity aluminum dish overnight (16 to24 h), handling with metal tongs.16.2 Place in a dessicator for at least 5 min. If the condi-tioned dish is not used within 24 h of cooling, repeat theconditioning process.16.3 Weigh a conditioned aluminum pan to the nearest0.0001 g, W1.16.4 Place the aluminum pan u
40、nder the heat lamp in a fumehood. The heat lamp should be positioned approximately 5 in.(12.7 cm) above the bottom of the aluminum dish. Slowly add100 mL of the solvent to the pan using a volumetric pipet.16.5 Turn on the heat lamp and evaporate until only a smallamount (about 1 mL) of liquid remain
41、s.16.6 Place the pan and contents in an oven at 105C for 10to 15 min.16.7 Remove the pan with tongs and place in a dessicatorfor at least 5 min to cool. Weigh the pan and contents W2.16.8 Calculate the nonvolatile matter (NVM) by the for-mula:PPM NVM 5W22 W1! X 1 000 000Density X 100!(5)where densit
42、y is the density of the solvent being analyzed.17. Precision and Bias217.1 The standard deviation of results of a single analystover different days was determined to be 1.9 ppm at a level of10 ppm nonvolatile matter17.2 The standard deviation of results from multiple labo-ratories over multiple days
43、 was determined to be 3.6 ppm at alevel of 10 ppm nonvolatile matter.17.3 Overall recovery for this method was 123.0 % fromapproximately 1 ppm to approximately 100 ppm nonvolatilematter.17.4 The lower quantification limit is approximately 1 ppm.18. Keywords18.1 halogenated organic solvents; nonvolat
44、ile matter; non-volatile residue; residue on evaporation2Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D26-1017.D2109 01 (2011)3ASTM International takes no position respecting the validity of any patent rights asserted in conne
45、ction 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 infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsi
46、ble 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 for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful co
47、nsideration 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 known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100
48、 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 ASTM 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/).D2109 01 (2011)4
