ASTM D5907-2003 Standard Test Method for Filterable and Nonfilterable Matter in Water《水中可过滤和不可过滤物质的标准测试方法》.pdf

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1、Designation: D 5907 03Standard Test Method forFilterable and Nonfilterable Matter in Water1This standard is issued under the fixed designation D 5907; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A num

2、ber in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This test method covers the determination of filterableand nonfilterable matter in drinking, surface, and saline waters,domestic and ind

3、ustrial wastes. The practical range of thedetermination of nonfilterable particulate matter is 4 to 20 000mg/L. The practical range of the determination of filterablematter is 10 to 20 000 mg/L.1.2 Since the results measured by this test are operationallydefined, careful attention must be paid to fo

4、llowing theprocedure as specified.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 to establish appro-priate safety and health practices and determine the applica-bility of regulatory limita

5、tions prior to use. For a specifichazard statement, see Section 9.2. Referenced Documents2.1 ASTM Standards:2D 596 Guide for Reporting Results of Analysis of WaterD 1129 Terminology Relating to WaterD 1192 Guide for Equipment for Sampling Water andSteam in Closed ConduitsD 1193 Specification for Rea

6、gent WaterD 2777 Practice for Determination of Precision and Bias ofApplicable Methods of Committee D-19 on WaterD 3370 Practices for Sampling Water from Closed ConduitsD 3856 Guide for Good Laboratory Practices in Laborato-ries Engaged in Sampling and Analysis of WaterD 5847 Practice for the Writin

7、g Quality Control Specifica-tions for Standard Test Methods for Water AnalysisE 319 Practice for the Evaluation of Single-Pan MechanicalBalancesE 898 Methods of Testing Top-Loading, Direct-ReadingLaboratory Scales and Balances3. Terminology3.1 Definitions: For definitions of other terms used in this

8、test method, refer to Terminology D 1129.3.2 Definitions of Terms Specific to This Standard:3.2.1 filterable matteralso commonly referred to as totaldissolved solids. It is that dissolved matter that is capable ofpassing through a glass fiber filter and dried to constant weightat 180C, as determined

9、 by following the procedures outlinedin this test method.3.2.2 nonfilterable matteralso commonly known as totalsuspended solids. It is that particulate matter that is retained ona glass fiber filter and dried to a constant weight at 103 to105C, as determined by following the procedures outlined inth

10、is test method.4. Summary of Test Method4.1 A well-mixed sample is filtered through a weighedstandard glass fiber filter. The suspended solids are retained onthe filter, which is dried at 105C and weighed. The increasedmass on the filter represents the nonfilterable matter.4.2 The filtrate from 4.1

11、may be used to determine thefilterable matter. The filtered sample (liquid phase) is evapo-rated to dryness and heated to 180C in a tared vessel to aconstant weight.5. Significance and Use5.1 Solids, both as filterable and nonfilterable matter, areimportant in the treating of raw water and wastewate

12、r, and inmonitoring of streams.5.2 Waste solids impose a suspended and settleable residuein receiving waters. Suspended and soluble materials provide amatrix for some biological slime and, in sufficient quantity,impair respiration of organisms. These solids may createnuisance slime beds and odors wh

13、ile imposing a long-termbiological oxidation load over limited receiving water areas.5.3 Knowledge of suspended and soluble materials is im-portant in treating raw water supplies. Knowledge of solidsloading can aid in determining the type or amount of treatment,or both, necessary to make the water a

14、cceptable for use. Suchinformation may also be used to determine acceptability of1This test method is under the jurisdiction of ASTM Committee D19 on Waterand is the direct responsibility of Subcommittee D19.05 on Inorganic Constituentsin Water.Current edition approved June 10, 2003. Published July

15、2003. Originallyapproved in 1996. Last previous edition approved in 1996 as D 5907 96a.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 Summar

16、y page onthe ASTM website.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.water after treatment. Too little treatment may not be desirableand excess treatment costs mo

17、ney.5.4 Stream monitoring is important for environmental rea-sons. Stream improvements, water pollution monitoring, masswasting, algal studies, and sediment loads are but a few of themany reasons streams are monitored.6. Interferences6.1 For some samples, chemical reactions may cause somematerials t

18、o change from one phase to another. For example, insome groundwaters, ferrous ions may form insoluble ferrichydroxides. Softened water high in carbonates may precipitatecalcium carbonate. In such cases, holding time may have acritical impact upon both the filterable and nonfilterable matter.Such sam

19、ples may have to be filtered in the field.6.2 This test method is not meant to include nonrepresen-tative particulates such as leaves, sticks, insects, fish, etc.Theseshould be removed before the analysis.6.3 Certain materials may be measured poorly, or not at all.Some materials may decompose or vol

20、atilize at the requiredtemperature. Other substances, such as glycerin or sulfuricacid, will remain liquid at the required temperature, givingvariable results. Oils and greases may present similar problemsand can end up in either the filterable or nonfilterable portion.6.4 Suspended solids samples h

21、igh in dissolved matter, suchas saline waters, brines, and some wastes, may be subject to apositive interference by the retention of dissolved matter, suchas salts and sugars, on the filter. Care must be taken in the finalrinsing of the filter so as to minimize this potential interferent.Additional

22、washing may be necessary.6.5 Clogging of the filter with too fine or too much materialwill prolong the filtering time and retain smaller particles thatwould normally pass through the filter, thus giving elevatedvalues to nonfilterable matter and low values to the filterablematter. Biological materia

23、l, such as algae, may also prolongfiltration time or plug the filter.6.6 Some samples may be hygroscopic, requiring prolongeddrying, extra careful desiccation, and rapid weighing. Forfilterable matter, samples highly mineralized or high in bicar-bonate may require careful and possibly prolonged dryi

24、ng. Forthe bicarbonate, the extended drying may be needed to ensurecomplete conversion to carbonate.6.7 Too much material retained on the filter may entrapwater, and may also require extended drying time for thesuspended solids. For filterable matter, excessive residue in thedish may cause the forma

25、tion of a water-trapping crust, givingelevated values.6.8 For some users, certain biological materials, such asalgae, slimes, insects, or other small crustaceans, may beconsidered to be positive interferences for nonfilterable matter.Modifications or adjustments may be needed to generate abetter val

26、ue.An example is determining chlorophyll content toestimate the amount of algae present. Such modifications maybe beyond the scope of this test method.7. Apparatus7.1 Glass Fiber Filters, without organic binder.3NOTE 1Although there is no organic binder in these filters, they maycontain a wet streng

27、th resin that is partially soluble. It is thereforeimportant to adequately prewash the filters as prescribed.7.2 Membrane Filter AssemblyAborosilicate glass, stain-less steel, or plastic funnel with a flat, fritted, or grid base so asto provide uniform support and filterable surface. The topsection

28、of the funnel shall fit over the edge of the filter toprovide a seal. The top should be removable to allow easyaccess for removing the filter. A Gooch crucible with a frittedbottom may be used in lieu of the funnel.7.3 Planchet or Pan, made of aluminum or stainless steel,capable of supporting the fi

29、lter when it is not on the filterassembly.7.4 Drying Oven, capable of maintaining a temperaturebetween 103 and 105C for nonfilterable matter and between178 and 182C for filterable matter.NOTE 2To prevent dust and sample from being blown around, it ispreferred that the oven for the particulate matter

30、 be of a gravity convectiontype. If this is not possible, samples should be shielded from the forced airof mechanical convection ovens.7.5 Analytical Balance, capable of measuring to the nearest0.1 mg.47.6 Vacuum Source.8. Reagents and Materials8.1 Purity of WaterUnless otherwise indicated, referenc

31、esto water shall be understood to mean reagent water conformingto Type I or II of Specification D 1193. Type III or IV may beused if they effect no measurable change in the blank orsample.9. Hazards9.1 Care must be taken to ensure filter funnels and filteringflasks are in a sound state. Any tiny nic

32、k, scratch, or weaknessin glass flasks or other apparatus can create a potential for animplosion hazard. Wrapping a flask is not adequate protectionin case of an implosion. It is recommended that a solid shield,such as a plexiglass cage, be placed around any filtering flask.10. Sampling10.1 Collect

33、the sample in accordance with the applicableASTM standard as follows: Specification D 1192 and PracticesD 3370.11. Procedure11.1 Prepare the glass fiber filters before use.3Millipore AP-40, Whatman 934-AH, Gelman type A/E, or equivalent, wasspecified for the round-robin.4The balance prescribed in th

34、is test method should be tested periodicallyaccording to Practice E 319 or Test Method E 898.D590703211.1.1 Place the glass fiber filter on the membrane filterassembly, or insert into the bottom of a suitable Goochcrucible, with the wrinkled surface up. While a vacuum isapplied, wash the disc with t

35、hree successive volumes of water.Each volume of water should be equal to 3 mL for each squarecentimetre of filterable surface area. For standard 47 mm filterholders with 35 mm diameter funnels, this would be 30 mL foreach wash for a total of 90 mL. Continue the vacuum until thefree water has been re

36、moved. Discard the washings.NOTE 3Proper washing is important for removing loose fiber and wetstrength resins. One 90-mL wash is not as effective as three 30-mLwashes.NOTE 4On some filters it may be difficult to tell which is the wrinkledside. Usually the opposite side has faint markings of the wire

37、 mesh usedto manufacture the filter mat.11.1.2 Skip 11.1.3 and 11.1.4 if only filterable matter isbeing determined.11.1.3 Release the vacuum and carefully remove the filterwith forceps. Place the filter on a planchet, and dry in an ovenat 103 to 105C for 1 h. Gooch crucibles with filter may behandle

38、d without the planchet.11.1.4 Remove from the oven and place in a desiccator untilcool. If the desiccation time exceeds 12 h, reheat and desiccateagain. Weigh the filter plus planchet to the nearest 0.1 mg justbefore using.After oven drying, the filter shall be handled onlywith forceps, and the plan

39、chet or crucible shall be handled onlywith forceps, tongs, or lint-free gloves.11.2 Preparation of the Evaporating Dish:11.2.1 If filterable matter is to be determined, heat a cleandish to 178 to 182C in an oven for 1 h. After removing fromthe oven, treat as in 11.1.3.NOTE 5The dish should be as sma

40、ll as practical to contain the volumeof the sample plus the rinses.The relative mass of the dish needs to be keptat a minimum in order to be able to measure small mass differences withany accuracy. This is because of the inherent difficulties of trying tocontrol temperature and moisture on a large m

41、ass within the requirementsof the test. For larger volumes, it may be more practical to evaporatesmaller increments, refilling the dish when dry until all the sample istransferred.NOTE 6The dish should be made of a material that is inert to thesample. Materials such as aluminum will oxidize when hea

42、ted with manyliquids, increasing the mass of the pan. Glass or light weight ceramicmaterial is generally preferred.11.3 Determine the proper sample volume.11.3.1 Sample volume determination for nonfilterable mat-ter.11.3.1.1 Start with a volume of sample equal to about 10mL/cm2of filterable surface

43、area. For the standard 47 mm filterholders with 35 mm diameter funnels, this would be about 100mL. If this fails to yield at least 2.5 mg of dry solids on thefilter, increase the sample volume until that mass is attained, avolume of 1 L is reached, or the “break point” in 11.3.1.3 isreached. Do not

44、exceed 200 mg on the filter.11.3.1.2 For other filter sizes, maintain at least 1 mg of drysolids per 4 cm2of filterable surface area, with a minimum of2.5 mg.11.3.1.3 If the filtration time exceeds 5 min, develop a“break-point” curve (see 11.3.3). This process needs to be doneonly when the character

45、 of a sample is unfamiliar or changes.11.3.2 Sample volume determination for filterable matter.11.3.2.1 Choose a sample volume to yield between 2.5 and200 mg. If more than 5 min is needed for the filtration, performthe “break point” determination as per 11.3.3.NOTE 7If the solids are expected to be

46、high, a known proportion ofthe total material, sample plus wash solution, that passed through the filtermay be used for the determination. For example, if 200 mL of sample wasfiltered and only 190 mL of liquid passed through the filter (with all freefilterable liquid passing through, leaving 10 mL o

47、f nonfilterable solidsretained on the filter), the total volume of filtrate would be 250 mL,including the wash water. If a 100-mL portion of the filtrate could be usedfor the filterable solids test, the final mass of dried solids weighed wouldhave to be divided by 0.4 to account for the 40 % proport

48、ion of the sampleused.11.3.3 Break-Point Determination:11.3.3.1 Place filter in the filtering apparatus. For thisprocedure, the filter needs no preparation. Add a small, knownvolume of sample that will filter rapidly and time how long ittakes to filter.11.3.3.2 Repeat 11.3.3.1, increasing the volume

49、 until it canbe determined at what point the filtration rate drops off rapidly.11.3.3.3 Plot the time versus the volume filtered. Select theproper volume as that just short of the time that a significantchange in filtration rate occurs. An example of a break pointcurve is shown in Appendix X1.NOTE 8If at least 2.5 mg of material cannot be retained on the filterbecause of plugging, a larger diameter filtration system is suggested.Fritted membrane style filter holders range in sizes up to 9 cm in diameter.11.3.4 Analyze sample volumes of less than 20 mL bydiluting 10