ASTM D1035-94

Standard Test Methods for Chemical Analysis of Fluor-Chrome-Arsenate-Phenol (Withdrawn 2000)

SCOPE
1.1 These test methods cover the determination of the chemical analysis of commercial fluor-chrome-arsenate-phenol.
1.1.1 Test Method D38 covers the sampling of wood preservatives prior to testing.  
1.2 The analytical procedures appear in the following order:  Sections Fluorine (calculated as F) 6 to 8 Arsenic (calculated as As2O3) 9 and 10 Chromium (calculated as CrO3) 11 and 12 Dinitrophenol or sodium pentachlorophenate 13 and 14
1.3 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.

General Information

• Status: Withdrawn
• Publication Date: 31-Dec-1993
• Withdrawal Date: 09-Apr-2000
• ICS: 71.080.90 - Phenols
• Technical Committee: D07 - Wood

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 1035 – 94 An American National Standard
Standard Test Methods for
Chemical Analysis of Fluor-Chrome-Arsenate-Phenol
This standard is issued under the fixed designation D 1035; 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 which is then diluted with water and titrated with a standard
solution of Potassium Bromate. Arsenic is calculated as As O .
2 5
1.1 These test methods cover the determination of the
3.3 Chromium—A diluted and chemically treated sample is
chemical analysis of commercial fluor-chrome-arsenatephenol.
reacted with an excess of ferrous ammonium sulfate. The
1.1.1 Test Method D 38 covers the sampling of wood
unreacted ferrous ammonium sulfate is titrated with a standard
preservatives prior to testing.
solution of potassium dichromate to determine the consumed
1.2 The analytical procedures appear in the following order:
chromium. Hexavalent chromium is calculated as CrO .
Sections
3.4 Phenol—The sample is dissolved in water, acidified
Fluorine (calculated as F) 6 to 8
Arsenic (calculated as As O ) 9 and 10
2 5 with sulfuric acid to free the phenolic compounds, and washed
Chromium (calculated as CrO ) 11 and 12
with ether to takeup the phenols. The ether is evaporated and
Dinitrophenol or sodium pentachlorophenate 13 and 14
the residue measured as phenols.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 4. Significance and Use
responsibility of the user of this standard to establish appro-
4.1 Fluor-Chrome-Arsenate-Phenol for use in the preserva-
priate safety and health practices and determine the applica-
tive treatment of wood must conform with Specification
bility of regulatory limitations prior to use.
D 1034.
2. Referenced Documents
5. Reagents
2.1 ASTM Standards:
5.1 Purity of Reagents—Reagent grade chemicals shall be
D 38 Test Methods for Sampling Wood Preservatives Prior
used in all tests. Unless otherwise indicated, it is intended that
to Testing
all reagents shall conform to the specifications of the Commit-
D 1033 Methods of Chemical Analysis of Chromated Zinc
tee on Analytical Reagents of the American Chemical Society,
Chloride
where such specifications are available. Other grades may be
D 1034 Specification for Fluor-Chrome-Arsenate-Phenol
used, provided it is first ascertained that the reagent is of
D 1193 Specification for Reagent Water
sufficiently high purity to permit its use without lessening the
accuracy of the determination.
3. Summary of Test Methods
5.2 Purity of Water—Unless otherwise indicated, references
3.1 Fluorine—Fluorine is removed by steam distillation
to water shall be understood to mean reagent water conforming
from an acidified sample. The distillate is neutralized and
to Specification D 1193.
titrated with a standard solution of Thorium Nitrate. Fluorine is
calculated as F. FLUORINE
3.2 Arsenic—A diluted sample is acidified with Hydrochlo-
6. Apparatus
ric and hypophosphorous acid to precipitate the arsenic. The
arsenic is volatilized by heating in the presence of sulfuric acid, 6.1 A suitable apparatus for the distillation of fluorine is
shown in Fig. 1.
7. Reagents
These test methods are under the jurisdiction of ASTM Committee D-7 on
Wood and are the direct responsibility of Subcommittee D07.06 on Treatments for
7.1 Potassium Permanganate Solution (saturated).
Wood Products.
7.2 Sodium Alizarin Sulfonate Indicator—Dissolve 0.05 g
Current edition approved April 15, 1994. Published June 1994. Originally
of sodium alizarin sulfonate in 100 mL of water.
published as D 1035 – 49. Last previous edition D 1035 – 87.
These methods are essentially the same as Sections 2, 5, 7, and 8 of the American
Wood-Preservers’ Association Standard Methods for Analysis of Water-Borne
Preservatives and Fire-Retardant Formulations (A2-84). Acknowledgment is made
Reagent Chemicals, American Chemical Society Specifications, American
to the American Wood Preservers’ Association for its development of the subject Chemical Society, Washington, DC. For suggestions on the testing of reagents not
matter covered in this standard. listed by the American Chemical Society, see Analar Standards for Laboratory
Annual Book of ASTM Standards, Vol 04.10. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Discontinued—See 1992 Annual Book of ASTM Standards, Vol 04.09. and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 11.01. MD.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 1035
the flow of steam from flask A so as to maintain a constant
volume of liquid in flask B and a boiling point of 140 to 145°C.
Distill until 300 mL of distillate are collected.
8.3 To 100 mL of the distillate, add 8 drops of sodium
alizarin sulfonate indicator solution. Adjust the acidity, using
NaOH solution and HCl (1 +199), until the solution is just acid
and the pink color is discharged. Add 1 mL of the buffer
solution and titrate with Th(NO ) solution to a persistent pink
3 4
color.
8.4 Calculation—Calculate the percentage of fluoride as
NaF, as follows:
F, % 5 @~AB 3 0.018!/0.4C# 3 100 (1)
where:
A 5 Th(NO ) solution required for titration of the 100-mL
3 4
aliquot of the sample, mL,
B 5 normality of the Th(NO ) solution, and
3 4
A—Florence flask, 2000-mL (A number of stills can be D—Thermometer
C 5 sample used, g.
operated from a single 2000-mL Florence flash)
B—Claissen flask, 250-mL E and
F—Pinchcocks
ARSENIC
C—Liebig condenser G—Bunsen burner
FIG. 1 Distillation Apparatus for Determination of Sodium 9. Reagents
Fluoride in Fluor-Chrome-Arsenate-Phenol
9.1 Hypophosphorous Acid (50 %).
9.2 Sulfuric Acid (sp gr 1.84).
9.3 Hydrochloric Acid (sp gr 1.19).
7.3 Sodium Hydroxide Solution (20 g/L)—Dissolve 2.0 g of
9.4 Methyl Orange Indicator Solution—Dissolve 0.1 g of
NaOH in 100 mL of water.
methyl orange in water and dilute to 100 mL.
7.4 Hydrochloric Acid (1 +199).
9.5 Standard Potassium Bromate Solution (0.1000 N)—
7.5 Buffer Solution—Dissolve 9.448 g of monochloroacetic
Dissolve 2.784 g of KBrO in water and dilute to 1 L in a
acid and 2.000 g of NaOH in 100 mL of water. 3
volumetric flask.
7.6 Thorium Nitrate, Standard Solution (0.1 N)—Dissolve
13.8 g of Th(NO ) ·4H O in water and dilute to 1 L.
3 4 2
10. Procedure
Standardize by titrating the fluorine obtained by distillation of
10.1 Transfer a weighed portion of the sample containing
100 % natural cryolite (3NaF·AlF ) or NaF, using the proce-
arsenic equivalent to about 0.15 g As O (Note, 8.1) to a
dure described in 8. 2 5
250-mL wide-mouth Erlenmeyer flask and dilute with water to
about 50 mL.
8. Procedure
10.2 Add 50 mL of HCl and 20 mL of H PO , mix
3 2
8.1 Transfer a weighed portion of the sample, equivalent to
thoroughly, and warm the solution on a steam bath until a
about 0.025 g of F (Note 1), to a 250-mL Cl
...