ASTM D1628-94(2000)

Standard Test Methods for Chemical Analysis of Chromated Copper Arsenate (Withdrawn 2006)

SCOPE
1.1 These test methods cover the chemical analysis of solid chromated copper arsenate and solutions of this material.
1.1.1 Test Method D 38 covers the sampling of wood preservatives prior to testing.  
1.2 The analytical procedures occur in the following order:  Sections Pentavalent arsenic (calculated as As2O5) 7 to 9 Copper (calculated as CuO) 10 to 13 Hexavalent chromium (calculated as CrO3) 14 to 16
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. Specific precautionary statements are given in 8.2, 12.1.2, and in accordance with the safety precautions section of Test Method D4278.
WITHDRAWN RATIONALE
These test methods cover the chemical analysis of solid chromated copper arsenate and solutions of this material.
Formerly under the jurisdiction of Committee D07 on Wood, these test methods were withdrawn without replacement in July 2006.

General Information

• Status: Withdrawn
• Publication Date: 09-Jan-2000
• Withdrawal Date: 12-Jul-2006
• ICS: 71.060.50 - Salts
• Technical Committee: D07 - Wood
• Drafting Committee: D07.06 - Treatments for Wood Products

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Please contact ASTM International (www.astm.org) for the latest information.
Designation:D1628–94 (Reapproved 2000)
Standard Test Methods for
Chemical Analysis of Chromated Copper Arsenate
This standard is issued under the fixed designation D 1628; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope D 1627 Methods for Chemical Analysis of Acid Copper
Chromate
1.1 These test methods cover the chemical analysis of solid
D 4278 Test Method for Wet Ashing Procedure for Prepar-
chromated copper arsenate and solutions of this material.
ing Wood Samples for Inorganic Chemical Analysis
1.1.1 Test Method D 38D38 covers the sampling of wood
preservatives prior to testing.
3. Summary of Test Methods
1.2 The analytical procedures occur in the following order:
3.1 Add 20 mL of tartaric acid solution to a 250-mL
Sections
Erlenmeyer flask, then add 2 mL of the ACA concentrate. The
Pentavalent Arsenic (calculated as As O ) 7-9
2 5 resulting solution should become light blue-green. Twenty
Copper (calculated as CuO) 10-13
millilitres of sodium bicarbonate solution is then added and the
Hexavalent Chromium (calculated as CrO ) 14-16
solution will turn light blue. Two millilitres of the starch
1.3 This standard does not purport to address all of the
indicator is added. To this solution, one drop of iodine solution
safety concerns, if any, associated with its use. It is the
from a buret is added. If the solution turns a dark blue and
responsibility of the user of this standard to establish appro-
remains, then the aeration is complete.
priate safety and health practices and determine the applica-
4. Significance and Use
bility of regulatory limitations prior to use. Specific precau-
tionary statements are given in 8.2, 12.1.2, and in accordance
4.1 These test methods test the completion of aeration
with the safety precautions section of Test Method
which is used to convert trivalent arsenic to pentavalent
D 4278D 4278.
arsenic.
2. Referenced Documents
5. Purity of Reagents
2.1 ASTM Standards:
5.1 Purity of Reagents—Reagent grade chemicals shall be
D38 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 onAnalytical Reagents of theAmerican Chemical Society,
Chloride
where such specifications are available. Other grades may be
D 1035 Test Methods for Chemical Analysis of Fluor-
used, provided it is first ascertained that the reagent is of
Chrome-Arsenate-Phenol
sufficiently high purity to permit its use without lessening the
D 1193 Specification for Reagent Water
accuracy of the determination.
D 1326 Methods for Chemical Analysis of Ammoniacal
5.2 Purity of Water—Unless otherwise indicated, references
Copper Arsenate and Ammoniacal Copper Zinc Arsenate
to water shall be understood to mean reagent water conforming
D 1625 Specification for Chromated Copper Arsenate
to Specification D 1193D 1193.
6. Sampling
These test methods are under the jurisdiction of ASTM Committee D-7 on
6.1 When the material to be sampled is a water solution, it
Wood and are the direct responsibility of Subcommittee D07.06 on Treatments for
Wood Products.
shall be mixed to ensure uniformity and the sample shall be at
Current edition approved July 15, 1994. Published September 1994. Originally
least 0.45 L and preferably 0.9 L. The sample shall be
published as D1628 – 59 T. Last previous edition D1628 – 90.
The analytical methods and sampling procedures are substantially the same as
those given in the American Wood-Preservers’ Association Standard Methods for
Analysis of Water-Borne Preservatives and Fire-Retardant Formulations (A2-82). Reagent Chemicals, American Chemical Society Specifications, American
Acknowledgment is made to the American Wood-Preservers’ Association for its Chemical Society, Washington, DC. For suggestions on the testing of reagents not
development of the subject matter covered in these test methods. 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 International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Please contact ASTM International (www.astm.org) for the latest information.
D1628–94 (2000)
representative and taken by a“ thief” or other device. The acid-washed asbestos, and washing the flask and precipitate
sample shall be collected and stored in properly closed thoroughly with water.
containers of glass or other suitable material. 8.4 Place the crucible containing the precipitate in the flask
6.2 When the material to be sampled consists of solids, a in which the precipitation was carried out. Discard the filtrate.
sample at least 2.3 kg in weight shall be taken from various Pour 10 mL of H SO into the flask and, while agitating, heat
2 4
points in the container or containers so that a representative over an open flame in a hood until dense white fumes are
sample is obtained. It shall be kept in an airtight container to evolved.
prevent changes in composition by reason of moisture absorp- 8.5 Allow the flask and contents to cool, and then add 100
tion or loss or chemical action of the air. mLof water very slowly and carefully, especially at first, since
6.3 The analytical procedures given in these test methods heat is generated during this addition. Next, add 5 mL of HCl
specify samples containing between 0.1 and 1.0 g of the and 2 drops of methyl orange indicator solution and titrate
ingredient to be determined. If the sample is solid, unless it is immediately with 0.1000 N KBrO solution.When the solution
dry and finely pulverized, it is preferable to weigh a larger becomes colorless, the end point has been reached.
sample than specified and dissolve this in a definite quantity of
9. Calculation
water from which aliquots containing the specified quantity
may be taken for analysis. Prepared samples or solutions
9.1 Calculate the percentage of pentavalent arsenic,As O ,
2 5
having a content of 10 to 20 g of solid preservative equivalent as follows:
per litre are usually convenient. Samples of solution from
As O,% 5 0.5746 A/B (1)
2 5
working tanks or plant equipment shall be filtered at a working
temperature immediately on obtaining and shall not be filtered where:
A = 0.1000 N KBrO solution required for titration of the
at the time the analysis is performed. Should any precipitate or
sample, mL, and
solid adhering to the container be present when the sample is
B = sample used, g.
analyzed, the solution and any such precipitate or solid shall be
thoroughly intermixed before analysis in order to obtain a
COPPER
proper sample.
NOTE 2—This procedure is essentially the same as the procedure for
ARSENIC
copper in Test Methods D 1326 and D 1627D 1326D 1627.
NOTE 1—This procedure is essentially the same as the procedure for
10. Reagents
arsenic Method D 1326D 1326.
10.1 Ammonium Hydroxide (sp gr 0.90)—Concentrated am-
7. Reagents
monium hydroxide (NH ·OH).
10.2 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
7.1 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
chloric acid (HCl). chloric acid (HCl).
10.3 Methanol.
7.2 Hypophosphorous Acid (50 %)—Concentrated hypo-
phosphorous acid (H PO ). 10.4 Potassium Chlorate-NitricAcid Mixture—Dissolve5g
3 2
ofpotassiumchlorate(KClO )in100mLofconcentratednitric
7.3 Methyl Orange Indicator Solution (0.1 g/L)—Dissolve
0.1 g of methyl orange in water and dilute to 1 L. acid (HNO , sp gr 1.42). Prepare this solution just before use
and do not save any surplus solution for use later.
7.4 Potassium Bromate, Standard Solution (0.1000 N)—
Dissolve 2.784 g of potassium bromate (KBrO ) in water and 10.5 Copper Foil or Shot.
10.6 Nitric Acid, concentrated (sp gr 1.42).
dilute to 1 L in a volumetric flask.
7.5 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric acid 10.7 Urea Solution, 5 %. Dissolve 5 g urea in 95 mL water.
10.8 Acetic Acid, glacial.
(H SO ).
10.9 Potassium Iodide Solution (200 g/L)—Dissolve 200 g
8. Procedure
of potassium iodide (KI) in water and dilute to 1 L.
10.10 Sodium Thiocyanate Solution (200 g/L)—Dissolve
8.1 Transfer a measured portion of the sample containing
arsenic equivalent to about 0.17 g of As O to a 250-mL 200 g of sodium thiocyanate (NaCNS) in water and dilute to 1
2 5
wide-mouthErlenmeyerflaskanddilutewithwatertoabout50 L.
mL.Add 50 mLof HCl and 20 mLof H PO , mix thoroughly, 10.11 Sodium Thiosulfate, Standard Solution (0.1 N)—
3 2
andwarmthesolutiononasteambathuntilaprecipitateforms. Dissolve 24.85 g of dry but not effloresced sodium thiosulfate
Boil gently for about 15 min. (Na S O ·5H O) and 1.0 g of sodium carbonate (Na ·CO )
2 2 3 2 2 3
8.2 Warning—If the sample being analyzed is a wood in water and dilute to 1 L.
sample digested with a perchloric acid mixture it now contains 10.11.1 Sodium thiosulfate solution prepared in accordance
perchloric acid and a strong reducing agent, hypophosphorus with 10.11 is usually close enough to 0.1 N and stable enough
acid. If it is evaporated too much, it may explode with to give reasonable service. However, on standing, particularly
dangerous violence. Do not boil longer than the specified time at elevated labor
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