ASTM D3804-02(2008)
(Test Method)Standard Test Method for Iron in Paint Driers by EDTA Method
Standard Test Method for Iron in Paint Driers by EDTA Method
SIGNIFICANCE AND USE
This test method may be used to confirm the stated content of a liquid iron drier soluble in isopropyl alcohol and manufactured for use in the coatings industry. The content determines activity level.
SCOPE
1.1 This test method covers the titrimetric determination of iron in liquid iron driers soluble in isopropyl alcohol and utilizes the disodium salt of ethylenediaminetetraacetic acid dihydrate (EDTA).
1.2 This test method is limited to the determination of the iron content of a liquid drier that does not contain other drier elements. This method is not applicable to drier blends.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: D3804 − 02 (Reapproved2008)
Standard Test Method for
Iron in Paint Driers by EDTA Method
This standard is issued under the fixed designation D3804; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 4. Significance and Use
1.1 This test method covers the titrimetric determination of 4.1 This test method may be used to confirm the stated
iron in liquid iron driers soluble in isopropyl alcohol and content of a liquid iron drier soluble in isopropyl alcohol and
utilizes the disodium salt of ethylenediaminetetraacetic acid manufactured for use in the coatings industry. The content
dihydrate (EDTA). determines activity level.
1.2 This test method is limited to the determination of the
5. Interferences
iron content of a liquid drier that does not contain other drier
5.1 All cations that can be titrated with EDTA in alkaline
elements. This method is not applicable to drier blends.
media interfere and must not be present in the sample or must
1.3 The values stated in SI units are to be regarded as
be masked.
standard. No other units of measurement are included in this
standard. 6. Reagents
1.4 This standard does not purport to address all of the
6.1 Purity of Reagents—Reagent grade chemicals shall be
safety concerns, if any, associated with its use. It is the
used in all tests. Unless otherwise indicated, it is intended that
responsibility of the user of this standard to establish appro-
all reagents shall conform to the specifications of the Commit-
priate safety and health practices and determine the applica-
tee onAnalytical Reagents of theAmerican Chemical Society,
bility of regulatory limitations prior to use.
where such specifications are available. Other grades may be
used, provided it is first ascertained that the reagent is of
2. Referenced Documents
sufficiently high purity to permit its use without lessening the
accuracy of the determination.
2.1 ASTM Standards:
D600Specification for Liquid Paint Driers
6.2 Purity of Water—Unless otherwise indicated, references
D1193Specification for Reagent Water
towatershallbeunderstoodtomeanreagentwaterconforming
E180Practice for Determining the Precision of ASTM
to Type II of Specification D1193.
Methods for Analysis and Testing of Industrial and Spe-
6.3 Ammonium Hydroxide (1+3)—Add 10 mL of concen-
cialty Chemicals (Withdrawn 2009)
trated ammonium hydroxide (NH OH, sp gr 0.90) to 30 mL
E300Practice for Sampling Industrial Chemicals
water.
3. Summary of Test Method 6.4 Buffer Solution—Add 350 mL of concentrated ammo-
nium hydroxide (NH OH) to 54 g of ammonium chloride
3.1 The liquid iron drier is diluted with isopropyl alcohol
(NH Cl) and dilute to 1 L with water.
andtheironchelatedwithexcessstandardEDTA.Thesolution
is buffered and the excess EDTAis titrated with standard zinc 6.5 EDTA, Standard Solution (0.01 M)—Weigh to 10 mg
chloride solution to the Eriochrome Black T end point. about3.73gofthedisodiumsaltofethylenediaminetetraacetic
acid dihydrate (EDTA), dissolve in water, and dilute to
approximately 1 L in a polyethylene or borosilicate glass
This test method is under the jurisdiction of ASTM Committee D01 on Paint
bottle.
andRelatedCoatings,Materials,andApplicationsandisthedirectresponsibilityof
6.6 Hydrochloric Acid (1+3)—Add 3 mL of concentrated
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
Current edition approved Feb. 1, 2008. Published February 2008. Originally
hydrochloric acid (HCl, sp gr 1.19) to 9 mL of water.
approved in 1979. Last previous edition approved in 2002 as D3804–02. DOI:
10.1520/D3804-02R08.
2 4
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Reagent Chemicals, American Chemical Society Specifications, American
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Standards volume information, refer to the standard’s Document Summary page on listed by the American Chemical Society, see Analar Standards for Laboratory
the ASTM website. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
The last approved version of this historical standard is referenced on and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
www.astm.org. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3804 − 02 (2008)
6.7 Eriochrome Black-T Indicator—Titrate 0.20 g of the 9.2 Place a few grams of the drier in a 50-mL Erlenmeyer
concentrated dye with 100 g of NaCl and store in a tightly flask fitted with a cork through which passes a dropping tube
stoppered jar. This mixture remains stable for several years. and rubber bulb (or medicine dropper) and obtain the total
weight. Weigh by difference to 0.5 mg, 0.18 to 0.22-g speci-
6.8 Isopropyl Alcohol (99.5%).
mens(8to12drops),into400-mLbeakers.Thisspecimensize
6.9 Zinc Chloride, Standard Solution (0.01 M)—Weigh to
is for driers of 6% iron content; adjust the size according to
0.5 mg about 0.65 g of zinc (Note 1) onto a glazed paper.
expected percent iron to contain about 0.2 mM of iron. Add
Transfertoa1-Lvolumetricflaskandadd25mLofdiluteHCl
100 mL of isopropyl alcohol and 3 mL 1+3 HCl to each
(7+18) (add 7 mL of concentrated acid (sp gr 1.19) to 18 mL
specimenandswirltomix.Addafewboilingaidsandheatthe
of water). Warm if necessary on a steam bath to dissolve
solutionjusttoboilingonahotplate;removeandcooltoroom
completely. Cool, dilute to the mark with water and mix
temperature in a water bath.
thoroughly. Calculate the exact molarity of this approximately
9.3 From a buret measure 40.0 mL of standard EDTA
0.01-M solution as follows:
solution into each beaker.
...
This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation:D3804–86 (Reapproved 1996) Designation: D 3804 – 02 (Reapproved 2008)
Standard Test Method for
Iron in Paint Driers by EDTA Method
This standard is issued under the fixed designation D 3804; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This test method covers the titrimetric determination of iron in liquid iron driers soluble in isopropyl alcohol and utilizes
the disodium salt of ethylenediaminetetraacetic acid dihydrate (EDTA).
1.2 Thistestmethodislimitedtothedeterminationoftheironcontentofaliquiddrierthatdoesnotcontainotherdrierelements.
This method is not applicable to drier blends.
1.3
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2.1 ASTM Standards:
D 600 Specification for Liquid Paint Driers
D 1193 Specification for Reagent Water
E 180 Practice for Determining the Precision ofASTM Methods forAnalysis andTesting of Industrial and Specialty Chemicals
E 300 Practice for Sampling Industrial Chemicals
3. Summary of Test Method
3.1 The liquid iron drier is diluted with isopropyl alcohol and the iron chelated with excess standard EDTA. The solution is
buffered and the excess EDTA is titrated with standard zinc chloride solution to the Eriochrome Black T end point.
4. Significance and Use
4.1 This test method may be used to confirm the stated content of a liquid iron drier soluble in isopropyl alcohol and
manufactured for use in the coatings industry. The content determines activity level.
5. Interferences
5.1 All cations that can be titrated with EDTA in alkaline media interfere and must not be present in the sample or must be
masked.
6. Reagents
6.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where
such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination.
6.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to
Type II of Specification D 1193.
This test method is under the jurisdiction of ASTM Committee D-1D01 on Paint and Related Coatings, Materials, and Applications and is the direct responsibility of
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
Current edition approved April 25, 1986.Feb. 1, 2008. Published June 1986.February 2008. Originally published as D3804–79.approved in 1979. Last previous edition
D3804–79.approved in 2002 as D 3804 – 02.
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. ForAnnualBookofASTMStandards
, Vol 06.04.volume information, refer to the standard’s Document Summary page on the ASTM website.
Annual Book of ASTM Standards, Vol 11.01.Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For
suggestions on the testing of reagents not listed by the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and
the United States Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 3804 – 02 (2008)
6.3 Ammonium Hydroxide (1+3)—Add 10 mL of concentrated ammonium hydroxide (NH OH, sp gr 0.90) to 30 mL water.
6.4 BufferSolution—Add 350 mLof concentrated ammonium hydroxide (NH OH) to 54 g of ammonium chloride (NH Cl) and
4 4
dilute to 1 L with water.
6.5 EDTA, Standard Solution (0.01 M)—Weigh to 10 mg about 3.73 g of the disodium salt of ethylenediaminetetraacetic acid
dihydrate (EDTA), dissolve in water, and dilute to approximately 1 L in a polyethylene or borosilicate glass bottle.
6.6 Hydrochloric Acid (1+3)—Add 3 mL of concentrated hydrochloric acid (HCl, sp gr 1.19) to 9 mL of water.
6.7 Eriochrome Black-T Indicator—Titrate 0.20 g of the concentrated dye with 100 g of NaCl and store in a tightly stoppered
jar. This mixture remains stable for several years.
6.8 Isopropyl Alcohol (99.5 %).
6.9 Zinc Chloride, Standard Solution (0.01 M)—Weigh to 0.5 mg about 0.65 g of zinc (Note 1) onto a glazed paper. Transfer
to a 1-L volumetric flask and add 25 mL of dilute HCl (7+18) (add 7 mL of concentrated acid (sp gr 1.19) to 18 mL of water).
Warm if necessary on a steam bath to dissolve completely. Cool, dilute to the mark with water and mix thoroughly. Calculate the
exact molarity of this approximately 0.01-M solution as follows:
M 5W/65.4 (1)
where:
M = molarity of ZnCl solution, and
2 2
W = zinc used, g.
65.4 = atomic weight of zinc.
NOTE 1—Zinc ribbon cut into small pieces with clean scissors is preferred. Granular (20 mesh) zinc requires several hours of heating on a steam bath
for complete solution. Store the zinc ribbon in a tightly sealed container to prevent the surface of the zinc from oxidizing.
7. Sampling
7.1 Take a small sample of liquid drier from bulk using the procedures in Practice E 300 appropriate for the size of container,
tanks and tank cars or drums and cans.
NOTE 2—Liquid dr
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