1、Designation: D 2109 01 (Reapproved 2006)e1Standard Test Methods forNonvolatile Matter in Halogenated OrganicSolvents and Their Admixtures1This standard is issued under the fixed designation D 2109; the number immediately following the designation indicates the year oforiginal adoption or, in the cas
2、e of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript 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.e1NOTERemoved researc
3、h report references in Sections 7, 10, and 13 editorially in March 2008.1. Scope1.1 These test methods 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 oradm
4、ixtures having less than 50 ppm nonvolatile matter; orwhere precision better than 610 ppm is required.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
5、halogenated organicsolvents or their admixtures (for example, methylene chloride,trichlorotrifluoroethane) 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
6、 in halogenated organic solvents and their admixturesand where precision better than 610 ppm is required.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 This st
7、andard 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. Terminology2.1 Definiti
8、ons 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 solids arepresent in the s
9、ample, 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 and nonvolatile residue ar
10、e 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 stability of the solvent.3.2 Thes
11、e 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) (Method D).4.4 Steam Bat
12、h (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 capacity, (MethodE).4.11 10
13、00-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 Solvents and Fire Extingu
14、ishing Agents and are the directresponsibility of Subcommittee D26.04 on Test Methods.Current edition approved June 1, 2006. Published June 2006. Originallyapproved in 1962 as D 2109 62 T. Last previous edition approved in 2001 asD 2109 01.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box
15、 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 or within 0.1 mgof the last weighing. Rinse a clean dry 1000-m
16、L 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 and flask on a steam bath.Adjust a ring support to hold the f
17、lask 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-free area.)5.2 Evaporate the 1000-mL sample to dryness. Remo
18、ve 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 dish should beplaced inside a water bath while on the hot plate
19、 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 matter and report in weightpercent or parts per million as foll
20、ows: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 weight ppm. Two suchvalues should be considered suspect (95 %
21、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 they differ by more than 4.6 weight ppm.TEST METHOD B8. Procedur
22、e8.1 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 andplace on a steam bath.8.2 Evaporate the sample to dryness as in
23、 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 desiccator and weigh the dish andcontents.9. Calculation9.1 Calcul
24、ate 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 difference betweenTest Method B and Test Methods A and C is the
25、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 determined.TEST METHOD C11. Procedure11.1 Dry a 125-mL capacity p
26、latinum (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 with the solvent to be tested.11.2 Measure 1000 mL of the sa
27、mple 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. Rinse theflask twice with a 15-mL portion of the sample ret
28、ained 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 hotplate. Protect the evaporating dish from externalcontamin
29、ation 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 parts permillion as follows:Nonvolatile matter, ppm by weight 5A!
30、 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. TwoD 2109 01 (2006)e12such values should be considered suspect (95 % confidencelevel) i
31、f 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 than 4.6 weight ppm.TEST METHOD D14. Procedure14.1 Weigh 100
32、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. Evaporation of the solvent must be carried out in a fumehood.14.2 Wh
33、ile 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 aluminum weighing dish on the hot plate andevaporate until
34、 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 W2.Itisnotnecessary to cool the dish in a dessicator.14.7 C
35、alculate 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 but not more than 30 min.14.8.2 When the dish is free of l
36、iquid, 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 to the oven for 30 min and proceed beginning with14.6.15. P
37、recision 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 multiple days was determined to be 2.2 ppm at alevel of 10 ppm n
38、onvolatile 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 capacity aluminum dish overnight (16 to24 h), handling with met
39、al 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 under the heat lamp in a fumehood. The heat lamp should be
40、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 remains.16.6 Place the pan and contents in an oven at 105C for 1
41、0to 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 density is the density of the solvent being analyzed.17. Precisi
42、on 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 was determined to be 3.6 ppm at alevel of 10 ppm nonvolat
43、ile 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; nonvolatile matter; non-volatile residue; residue on evaporation2S
44、upporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D261017.D 2109 01 (2006)e13ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of
45、 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 responsible technical committee and must be reviewed every five
46、 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 consideration at a meeting of theresponsible technical co
47、mmittee, 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 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).D 2109 01 (2006)e14
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