1、Designation: D5547 95 (Reapproved 2017)Standard Test Method forClay and Zeolite in Powdered Laundry Detergents by AtomicAbsorption1This standard is issued under the fixed designation D5547; the number immediately following the designation indicates the year oforiginal adoption or, in the case of rev
2、ision, 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.1. Scope1.1 This test method covers atomic absorption tests appli-cable to powdered laundry detergents containi
3、ng clay andzeolite.21.2 The values stated in SI units are to be regarded as thestandard.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
4、 and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:3E180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals (Withdrawn 2009)43. Summary of Test Method3.1 The test sample
5、 is fused with lithium metaborate,dissolved in acid, its silicon and aluminum content measuredby atomic absorption, and the silicon/aluminum (Si/Al) ratiocalculated. The clay and zeolite content of the test sample iscalculated from the Si/Al ratio of the test sample and the Si/Alratio of the clay an
6、d zeolite expected in the test sample.4. Interferences4.1 Materials other than clay and zeolite that contain siliconor aluminum, or both, will interfere.5. Principle5.1 Clay and zeolite contain silicon and aluminum at differ-ent relative levels.5The silicon/aluminum ratio is then ameasure of the rel
7、ative level of clay and zeolite in detergentpowders. That is, detergent powders with a Si/Al ratio match-ing clay or zeolite contain only clay or zeolite, respectively.Detergent powders with Si/Al ratio falling between the Si/Alratio of clay and zeolite contain both clay and zeolite.5.2 This test me
8、thod is based on the linear relationshipbetween the relative composition (or ratio) of clay/zeolite indetergent powders and the Si/Al ratio of such detergents.5.3 A calibration equation is derivable, therefore, from justtwo experimental points: the Si/Al ratio of the zeolite standard(100 zeolite, 0
9、% clay) and the Si/Al ratio of the clay standard(0 % zeolite, 100 % clay).6. Apparatus6.1 Suitable Atomic Absorption Spectrophotometers, fittedwith a nitrous oxide-acetylene burner and aluminum andsilicon hollow cathode source lamps.6.2 Nitrous Oxide and Acetylene Tanks, with suitable regu-lators.6.
10、3 Muffle Furnace, capable of reaching 1000C.6.4 Analytical Balance.6.5 Fisher Burner or Equivalent.6.6 20-mL or Larger Platinum Crucibles.6.7 Platinum-tip Tongs.6.8 25-mL Buret.6.9 100-mL and 200-mL Polypropylene Volumetric Flasks.6.10 10-mL and 25-mL Graduated Cylinders.6.11 150-mL Plastic Beakers.
11、6.12 Magnetic Stirrer and Magnetic Stirring Bars.6.13 Blender, such as Waring6or Osterizer7or an industriallab model, or a mortar and pestle, if a blender is not available.1This test method is under the jurisdiction of ASTM Committee D12 on Soapsand Other Detergents and is the direct responsibility
12、of Subcommittee D12.12 onAnalysis and Specifications of Soaps, Synthetics, Detergents and their Components.Current edition approved Jan. 1, 2017. Published February 2017. Originallyapproved in 1994. Last previous edition approved in 2009 as D5547 95(2009).DOI: 10.1520/D5547-95R17.2Silicon and alumin
13、um measurements are by atomic absorption in this testmethod. ICP can be used to make such measurements as well.3For 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 s
14、tandards Document Summary page onthe ASTM website.4The last approved version of this historical standard is referenced onwww.astm.org.5The Si/Al ratio is usually about 1 in zeolites and about 3 in clays.6Waring blenders are available commercially.7Osterizer blenders are widely available commercially
15、.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of Inte
16、rnational Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.17. Reagents7.1 Purity of ReagentsReagents grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents conform to the specific
17、ations of the Committee onAnalytical Reagents of the American Chemical Society, wheresuch specifications are available.8Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.7.2 Pu
18、rity of WaterUnless otherwise indicated, referenceto water shall be understood to mean distilled water or water ofequal purity.7.3 Aluminum Standard, 1000 g Al/mL9or equivalent.7.4 Silicon Standard, 1000 g Si/mL.97.5 Potassium Chloride, Baker-analyzed reagent or equiva-lent.7.6 Potassium Chloride So
19、lution (1 %)Dissolve1gofpotassium chloride in 100 mL of distilled water. Mix well andstore in plastic container.7.7 Concentrated Hydrochloric Acid, Baker-analyzed re-agent or equivalent.7.8 Hydrochloric Acid Solution (1 + 1)Mix equal parts ofconcentrated HCl and distilled water by volume. Mix well a
20、ndstore in plastic container.7.9 Potassium Iodide, Baker-analyzed reagent or equiva-lent.7.10 Lithium Metaborate SPEX Grade, Special for Fu-sions.107.11 Zeolite StandardThe same material expected in thetest sample, to be used as standard.7.12 Clay StandardThe same material expected in the testsample
21、, to be used as standard.8. Instrumental Conditions8.1 Following the instrument manufacturers instructions,set up the atomic absorption instrument as follows:To measure Aluminum To measure SiliconWavelength, nm 309.3 251.6Range UV UVSlit, nm 0.2 0.2Flame Nitrous oxide-acetylene. Nitrous oxide-acetyl
22、ene.Rich, red. Strongly reducing red cone 23cm high with yellow outeredge.9. Procedure9.1 Determination of Aluminum:9.1.1 Accurately weigh 0.1 g (to the nearest 0.1 mg) ofzeolite standard (the same material expected in the test sample)into a clean, dry, platinum crucible. Also accurately weigh 0.2g
23、of clay standard (the same material expected in the testsample) into another clean, dry, platinum crucible.9.1.2 Grind a representative powdered detergent test samplein a blender to a fine, homogenous powder. (If a blender is notavailable, use a mortar and pestle).9.1.3 Accurately weigh 0.3 g (to th
24、e nearest 0.1 mg) of theground test sample(s) into still another clean, dry, platinumcrucible.9.1.4 Add2g(60.1 g) of lithium metaborate to eachplatinum crucible, and mix the contents with a plastic rod.9.1.5 Place the crucibles containing the mixtures in a coolmuffle furnace and turn on the heat. Wh
25、en the temperaturereaches 1000C, maintain heat for at least 5 additional min.NOTE 1The sample will ignite and splatter if placed in a hot furnace.If it is not possible to start with a cool furnace, gently char the sample witha Fisher burner first, avoiding ignition, then place in the furnace.9.1.6 P
26、lace 90 mL of distilled water into 150-mL plasticbeakers. (Use as many beakers as there are standards andsamples).9.1.7 Add a magnetic stirring bar to each beaker, and placeon a magnetic stirrer. Mix rapidly to make the water swirl inthe beaker, but do not allow anything to splash out. Thisapparatus
27、 should be near the furnace containing the ashedstandards and sample(s).9.1.8 Using platinum-tip tongs, remove one crucible at atime from the furnace, and immediately place over a Fisherburner flame without allowing the melted sample to solidify.9.1.9 Add about 2 mg (a pinch on the end of a spatula)
28、 ofpotassium iodide (KI) to the melted sample. A molten ball willform. Roll the ball around the inside of the dish to pick up anydroplets or particles. The KI releasing agent is volatile, and itis necessary to carry out this step rather quickly (about 2 min).If the ball collapses and flows into the
29、dish, start again byadding fresh KI.9.1.10 Drop each molten ball quickly into the swirling waterof each plastic beaker.NOTE 2Precaution: Use face shield and protective clothing.9.1.11 Add 20 mL of 1 + 1 HCl and 20 mL of 1 %potassium chloride solution and mix until completely dis-solved. Quantitative
30、ly transfer to a 200-mL plastic volumetricflask with distilled water. Dilute to volume and mix well.9.1.12 Using a buret, add 5, 7.5, and 10 mL of 1000-ppmaluminum standard into 3 separate 100-mL plastic volumetricflasks. These standards contain 50, 75, and 100 g Al/mLrespectively. (Make these stand
31、ards fresh each day).9.1.13 Add 10 mL 1 + 1 HCl, 10 mL 1 % KCl, and1goflithium metaborate to each flask. Dilute to volume withdistilled water and mix until completely dissolved.9.1.14 Prepare a reagents blank.9.1.15 Set up the atomic absorption instrument as describedin 8.1.9.1.16 Zero the instrumen
32、t with the reagents blank. Measurethe absorbance of the aluminum standards, the zeolite standard,the clay standard and the test sample at 309.3 nm. Repeat the8Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reag
33、ents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.9Available from Fisher Scientific Co., Fairlawn, NJ 07410.1
34、0Available from SPEX Industries, Box 798, Metuchen, NJ 08840.D5547 95 (2017)2measurement three more times for each flask and calculate theaverage absorbance. Save the solutions, except the aluminumstandards, for silicon determination in 9.2.9.1.17 Prepare a standard curve by plotting the averageabso
35、rbance versus concentration in g/mL of each aluminumstandard.9.1.18 Determine the concentration of aluminum in the testsample(s) by comparing the average absorbance to the standardcurve and reading aluminum concentration in g/mL directly.NOTE 3This test method describes manual data gathering andcalc
36、ulation from a calibration curve so that the technique can be carriedout using all atomic absorption units. It is acceptable to use the automaticconcentration modes in modern atomic absorption units if so equipped.9.1.19 Calculation:C 3200wt. 3100005 % aluminum (1)where:C = aluminum concentration (g
37、/mL),200 = final dilution in mL,wt. = weight of zeolite and clay standards, and testsample(s), in g, and10 000 = conversion factor, g/g to percent.9.2 Determination of Silicon:9.2.1 Pipet 5, 10, and 15 mL of 1000-ppm silicon standardinto three separate 100 mL plastic volumetric flasks.9.2.2 Add 10 m
38、L 1 + 1 HCl, 10 mL 1 % KCl, and1goflithium metaborate to each flask. Dilute to volume withdistilled water and mix until completely dissolved. Thesestandards contain 50, 100, and 150 g Si/mL respectively.(Make these standards fresh each day.)9.2.3 Prepare a reagents blank and dilute with distilled wa
39、ter50.0 mL of the clay standards from 9.1 to 100.0 mL in a100-mL plastic volumetric flask.9.2.4 Set up the atomic absorption instrument as describedin 8.1.9.2.5 Zero the instrument with the reagents blank. Measurethe absorbance of the silicon standards at 251.6 nm. Measure,also at 251.6 nm, the abso
40、rbance of the zeolite standard, theclay standard, and the test sample(s) from 9.1. Repeat themeasurement three more times for each flask and calculate theaverage absorbance.9.2.6 Prepare a standard curve by plotting the averageabsorbance versus concentration in g/mL of each siliconstandard.9.2.7 Det
41、ermine the concentration of silicon in the testsample(s), the zeolite standard, and the clay standard bycomparing the average absorbance to the standard curve andreading the silicon concentration in g/mL directly.NOTE 4This test method describes manual data gathering andcalculation from a calibratio
42、n curve so that the technique can be carriedout using all atomic absorption units. It is acceptable to use the automaticconcentration modes in modern atomic absorption units if so equipped.9.2.8 Calculation:C 3200wt. 3100005 % silicon (2)where:C = silicon concentration from curve (g/L),200 = final d
43、ilution in mL,wt. = weight of zeolite and clay standards and testsample(s), in g, and10 000 = conversion factor, g/g to percent.10. Calculation of Percent Clay and Percent Zeolite inTest Samples10.1 Calculate the Si/Al ratio for the clay standard, thezeolite standard, and the test sample(s) from per
44、cent aluminumand percent silicon obtained in 9.1 and 9.2, respectively.10.2 Derive the equation of the straight line, y=mx+c,connecting the points:x1, y15 Si/AlC!, 0 (3)x2, y25 Si/AlZ!, 100where:Si/Al( C) = Si/Al ratio of clay standard,Si/Al( Z) = Si/Al ratio of zeolite standard,0 = concentration of
45、 zeolite in clay standard, and100 = concentration of zeolite in zeolite standard.10.3 Calculate the relative level of zeolite in the testsample(s) using the equation from 10.2 and the Si/Al ratio ofthe test sample(s) from 10.1:yRLZ! 5 mx1c (4)where:y(RLZ) = relative level of zeolite in the test samp
46、le,m = slope of the line (10.2),x = Si/Al ratio of test sample, andc = intercept of the line (10.2).10.4 Percent Zeolite in Test Sample:ATS!RLZ!AZ!5 % zeolite (5)where:ATS = percent aluminum in test sample (9.1),RLZ = relative level of zeolite in test sample (10.3), andAZ = percent aluminum in zeoli
47、te standard.10.5 Percent Clay in Test Sample:ATS!100 2 RLZ!AC!5 % clay (6)where:ATS = percent aluminum in test sample (9.1),RLZ = relative level of zeolite in test sample (10.3), andAC = percent aluminum in clay standard.10.6 Sample Calculation for a Typical Clay, Zeolite, andPowdered Detergent:10.6
48、.1 Experimental Results:ClaystandardZeolitestandardPowderdetergent% Aluminum 8.8 16 3.3% Silicon 27.3 17.6 5.4Si/Al ratio 3.1 1.1 1.64D5547 95 (2017)310.6.1.1 Using the points x1, y1= 3.1, 0; x2, y2= 1.1, 100,the equation of the line is:y 5250x1155 (7)10.6.1.2 Relative Level of Zeolite (RLZ) in Dete
49、rgent Pow-der:y 5250!1.64!1155 5 73 (8)10.6.1.3 Percent Zeolite in Detergent Powder:ATS!RLZ!AZ!53.3!73!16!5 15.1 (9)10.6.1.4 Percent Clay in Detergent Powder:ATS!100 2 RLZ!AC!53.3!100 2 73!8.8!5 10.1 (10)11. Precision and Bias11.1 Six laboratories collaborated in analyzing two powderdetergents (A and B). See Table 1.11.2 The standard deviations for clay, covering the 5.2 to9.9 % clay range, and the standard deviations for zeolite,covering the 19.6 to 28.9 % zeolite range, were pooled. SeeTable 1.11.3 The following criteria should b
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