1、Designation: D 2109 01 (Reapproved 2006)Standard 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 case
2、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.1. Scope1.1 These test
3、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 oradmixtures having less than 50 ppm nonvolatile matter; orwhere precision better than 610 ppm is re
4、quired.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,trichlorotrifl
5、uoroethane) 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
6、 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 standard does not purport to address all of thesafety concerns, if any, associated with its use.
7、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 Definitions of Terms Specific to This Standard:2.1.1 The term nonvolatile matter should not be construe
8、das 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 sample, they should be removed by filtration ordecantation prior to beginning this test method.
9、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 are inter-changeable terms.3. Significance and Use3.1 Nonvolatile matter in solvents can adversel
10、y 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 These test methods can be used to establish manufac-turing and purchasing specifications.4. Apparat
11、us4.1 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 Bath (or hot plate).4.5 Hot Plate, (Method D).4.6 Heat Lamp, 250 W, (Method E).4.7 Analytical Bala
12、nce, 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 1000-mL Volumetric Flask (Test Method A).4.12 100-mL Volumetric Pipet (Test Method B and E).4.13
13、1000-mL Graduated Cylinder (Test Method C).4.14 1500-mL Erlenmeyer Flask (Test Method C).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
14、weighing. Rinse a clean dry 1000-mL volumetric1These test methods are under the jurisdiction of ASTM Committee D26 onHalogenated Organic Solvents and Fire Extinguishing Agents and are the directresponsibility of Subcommittee D26.04 on Test Methods.Current edition approved June 1, 2006. Published Jun
15、e 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 C700, West Conshohocken, PA 19428-2959, United States.flask with the solvent and fill to the 1000-mL mark with thesolvent to be tested. I
16、nvert 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 flask so the mouth of the flaskis approximately 25 mm above the bottom of the evaporatingdish. T
17、hus 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. Remove thedish from the steam bath with metal tongs and blot the outsideof the dish with lint-free
18、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 to prevent the samplefrom reaching temperatures exceeding 105C.5.3 Place the dish and contents
19、 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 follows:Nonvolatile matter, ppm by weight 5A! 106!B! 1000!5A! 1000!B!(1)where:A = grams of residue,
20、 andB = density of sample.7. Precision and Bias27.1 Repeatability (Single Analyst)The standard deviationof results has been estimated to be 0.2 weight ppm. Two suchvalues should be considered suspect (95 % confidence level) ifthey differ by more than 0.7 ppm.7.2 Reproducibility (Multilaboratory)The
21、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. Procedure8.1 Dry a 125-mL capacity platinum (or high-silica glass)evaporating dish in an oven at 105 6
22、 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 Section 5 (seeNote 1 and Note 1). Remove the dish from the steam bath withmetal tongs and blo
23、t 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 Calculate the nonvolatile matter and report in weightpercent as follows:Nonvolatile matter, ppm by w
24、eight 5A! 100!B! 100!5A!B!(2)where:A = grams of residue, andB = density of sample.10. Precision and Bias210.1 PrecisionAs the only significant difference 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 t
25、en 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 platinum (or high-silica glass)evaporating dish in an oven at 105C and cool in a desiccator.Re
26、peat 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 sample into the cleanedgraduate and transfer 970 mL of it into the clean Erlenmeyerflask. Evapo
27、rate 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 retained in thegraduate (see Note 2). Add the rinsings to the evaporating dish.NOTE 2All of the
28、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 externalcontamination and do not exceed 60C (140F). When evapo-ration is complete, dry the evaporating dish i
29、n 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! 106!B! 1000!5A! 1000!B!(3)where:A = grams of residue, andB = density of sample.13. Precision
30、 and Bias213.1 Repeatability (Single Analyst)The standard devia-tion of results has been estimated to be 0.2 weight ppm. Twosuch values 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
31、 been estimated to be 1.0 weight ppm. Two2A research report is available from ASTM headquarters. Request RR:D261017.D 2109 01 (2006)2such values should be considered suspect (95 % confidencelevel) if they differ by more than 4.6 weight ppm.TEST METHOD D14. Procedure14.1 Weigh 100 g of sample on a to
32、p 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 While the sample is e
33、vaporating, 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 only a small amoun
34、t 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 Calculate the nonvol
35、atile 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 liquid, remove it fr
36、om 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. Precision and Bias21
37、5.1 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 nonvolatile matter.1
38、5.3 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 metal tongs.16.2 Place
39、 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 positioned approxim
40、ately 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 10to 15 min.16.7 Rem
41、ove 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. Precision and Bias217.1 Th
42、e 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 nonvolatile matter.17.3 Ove
43、rall 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 evaporationD 2109 01 (2006)3ASTM
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47、n 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)4
