ASTM D5584-94(2000)

Standard Test Methods for Chemical Analysis of Ammoniacal Copper Quat, Type B (ACQ-B) (Withdrawn 2006)

SCOPE
1.1 These test methods cover the determination of the chemical analysis of commercial solutions of ammoniacal copper quat Type B (ACQ-B).  
1.2 The analytical procedures appear in the following order: Ammonia Quat (Didecyldimethylammonium chloride) Copper (calculated as CuO)
1.3 The values stated in SI units are to be regarded as the 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.
WITHDRAWN RATIONALE
These test methods cover the determination of the chemical analysis of commercial solutions of ammoniacal copper quat Type B (ACQ-B).
Formerly under the jurisdiction of Committee D07 on Wood, these test methods were withdrawn without replacement in July 2006.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• Status: Withdrawn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: 11-Jul-2006
• ICS: 71.100.50 - Wood-protecting chemicals
• 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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D5584–94 (Reapproved 2000)
Standard Test Methods for
Chemical Analysis of Ammoniacal Copper Quat, Type B
(ACQ-B)
This standard is issued under the fixed designation D 5584; 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 acid solution forming ammonium borate. This solution is
titrated against 0.2 N sulfuric acid. The normality of any
1.1 These test methods cover the determination of the
unreacted sulfuric acid solution is then determined by titration
chemical analysis of commercial solutions of ammoniacal
with standardized NaOH solution.
copper quat Type B (ACQ-B).
3.2 Quat in Solution—The concentration of quaternary
1.2 The analytical procedures appear in the following order:
ammonium compounds in ACQ-B concentrate and working
Ammonia
solutions can be determined by titration using a number of
Quat (Didecyldimethylammonium chloride)
Copper (calculated as CuO)
procedures. Two of the possible methods are provided here.
The first involves a two-phase (chloroform/water) titration.
1.3 The values stated in SI units are to be regarded as the
Sodium lauryl sulfate is used as the titrant and methylene blue
standard.
as the color indicator.The end point of the titration is indicated
1.4 This standard does not purport to address all of the
by a color change in the organic layer from colorless to light
safety concerns, if any, associated with its use. It is the
blue. The second procedure involves a single-phase titration.
responsibility of the user of this standard to establish appro-
After an initial neutralization step, ACQ-B solutions are
priate safety and health practices and determine the applica-
titrated against sodium tetraphenylborate using 2, 7
bility of regulatory limitations prior to use.
-dichlorofluorescein as the color indicator. The end point is
2. Referenced Documents
indicated by a solution color change from purple to green.
3.3 Quat in Wood—Two alternate test methods are pro-
2.1 ASTM Standards:
vided. The first procedure is a two-phase titrimetric method
D 1193 Specification for Reagent Water
similar to that used for ACQ-B solutions. A high performance
D 1628 Test Methods for Chemical Analysis of Chromated
liquidchromatography(HPLC)methodisalsoavailable.Inthe
Copper Arsenate
HPLC procedure a treated wood sample is ground to pass a
D 5654 Specification forAmmoniacal Copper Quat Type B
30-mesh screen and then extracted with acidified ethanol. An
(ACQ-B)
aliquot of this extract is filtered and then analyzed using a
2.2 A WPA Standards:
HPLC equipped with a Partisil SCX ion exchange column and
AWPAA2-92 StandardMethodsforAnalysisofWaterborne
a UV detector set at 262 nm. Benzyltrimethylammonium
Preservatives and Fire Retardant Formulations
chloride is added to the HPLC mobile phase to allow indirect
AWPA A9-90 Standard Method for Analysis of Treated
UV detection of DDAC type quats.
Wood and Treating Solutions by X-ray Spectroscopy
3.4 Copper in Solution or Wood—A variety of methods is
AWPA A11-83 Standard Method for Analysis of Treated
available for determining the copper content in ACQ-B solu-
Wood and Treating Solutions by Atomic Absorption
tion concentrates, work solutions, and wood. X-ray fluores-
Spectroscopy
cence is the most practical method for most wood treatment
3. Summary of Test Methods
operations. The procedures involved in this technique are
described inAWPAStandardA 9-90.An alternative procedure
3.1 Ammonia in Solution—Ammonia is freed from a caustic
uses atomic absorption spectroscopy as outlined in AWPA
solution of the sample by distillation and absorbed in a boric
Standard A-11-83. Copper in solution can also be determined
titrimetrically using the procedure described in Test Methods
These test methods are under the jurisdiction of ASTM Committee D-7 on
D 1628.
Wood and are the direct responsibility of Subcommittee D07.06 on Treatment for
Wood Products.
4. Significance and Use
Current edition approved July 15, 1994. Published September 1994.
Annual Book of ASTM Standards, Vol 11.01.
4.1 Ammoniacal copper quat Type B for use in the preser-
Annual Book of ASTM Standard, Vol 04.10.
vative treatment of wood must conform with Specification
Available from theAmericanWood Preservers’Association, P.O. Box 286, MD
D 5654.
21163.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D5584
5. Reagents 9. Procedure
5.1 Purity of Reagents—Reagent grade chemicals shall be
9.1 Assemble the apparatus as described above but do not
used in all tests. Unless otherwise indicated, it is intended that
connectthe500-mLKjeldahlflask.Placeapproximately75mL
all reagents shall conform to the specifications of the Commit-
of the boric acid solution in the 500-mL Erlenmeyer flask, add
tee onAnalytical Reagents of theAmerican Chemical Society,
four to five drops of bromocresol green indicator, and position
where such specifications are available. Other grades may be
the Erlenmeyer flask so that the tip of the condenser adaptor
used, provided it is first ascertained that the reagent is of
just dips into the boric acid solution.
sufficiently high purity to permit its use without lessening the
9.2 Place the sample for analysis in the Kjeldahl flask.
accuracy of the determination.
Dilute with distilled water to a volume of about 200 mL. Add
5.2 Purity of Water—Unless otherwise indicated, references
afewglassbeadstopreventbumping.Add5.0gofmagnesium
to water shall be understood to mean reagent water conforming
oxide and immediately attach the flask to the rest of the
to Specification D 1193.
apparatus by means of the rubber stopper on the spray trap.
DETERMINATION OFAMMONIA IN AMMONIACAL 9.3 After making sure that all connections are tight, and the
COPPER QUAT TYPE B (ACQ-B) FORMULATIONS
tip of the condenser adaptor is just below the surface of the
boric acid solution, commence heating the contents of the
6. Scope
Kjeldahl flask.
6.1 This test method is suitable for the detection of ammo-
9.4 Distill off about 150 mL of liquid. Adjust the height of
nia in solution provided that the sample analyzed contains
the Erlenmeyer flask throughout the distillation so that the tip
ammonia or ammonium in amounts approximating but not
of the condenser adaptor is always under, but near, the surface
exceeding 0.15 g NH or NH .
3 4 of the boric acid solution in the receiving vessel.
9.5 When the distillation is complete, lower the receiving
7. Apparatus
vessel and remove the heat source. Wash down the condenser
7.1 The apparatus consists of a 500-mL Kjeldahl flask to
tubeandadaptorintothereceivingvessel,usingdistilledwater.
which is attached a spray trap by means of a rubber stopper.
9.6 Titrate the ammonium borate solution so formed with
The spray trap can be found under “Kjeldahl distillation
standard 0.2 N sulfuric acid.
apparatus” in equipment catalogs where it is referred to as a
9.7 For standardization of sodium hydroxide solution,
“bulb.” The trap returns liquid to the distillation flask and
weigh two portions of potassium acid phthalate 1.6000 6
permits vapor to pass to a water-jacket condenser that directs
0.1000 g, transferring each to 500 mL Erlenmeyer flasks.
the condenser vapor downwards, then through a condenser
Dissolve in 100 mL freshly boiled and cooled water, adding
adaptor, into a 100-mL Erlenmeyer flask.
two drops phenolphthalein. Titrate with the sodium hydroxide
solution until a faint permanent pink color appears. Duplicate
8. Reagents
titrations should yield normalities within 0.0005 N.
8.1 Bromocresol Green Indicator , 0.1 % solution—
9.8 For standardization of the sulfuric acid solution, pipet
Dissolve1.0gbromocresolgreenin1.5mL0.1normalsodium
exactly 25 mL of the sulfuric acid solution into a 250-mL
hydroxide and dilute to 100 mL with distilled water.
Erlenmeyer flask. Add two drops of phenolphthalein indicator
8.2 Magnesium Oxide Powder.
and titrate with the standardized sodium hydroxide solution
8.3 Potassium Acid Phthalate, primary standard grade.
8.4 Boric Acid Solution, 4 %—Dissolve 40 g boric acid in until a faint permanent pink color appears. Duplicate titrations
960 mL distilled water. should agree to within 0.10 mL. Record the average.
8.5 Phenolphthalein Indicator, 1.0 % solution—Dissolve
1.0 g phenolphthalein in 10 mL ethyl alcohol (such as J. T.
10. Calculation
Baker, No. 9400 alcohol, reagent).
10.1 Normality of Sodium Hydroxide:
8.6 Sulfuric Acid Solution, 0.2 N—Place about 10 mL
g Potassium acid phthalate
distilled water in a 1000-mL volumetric flask, add 6.6 mL
mL NaOH 3 0.2042
concentrated sulfuric acid and cool to 20°C. Dilute to 1 Lwith
distilled water. (See standardization procedure below.)
10.2 Normality of Sulfuric Acid:
8.7 Sodium Hydroxide Solution, 0.2 N— Dissolve 8.1 g
normality of NaOH 3 mL NaOH
sodium hydroxide in CO -free distilled water, cool to room
temperature and dilute to 1 L with CO -free distilled water.
10.3 Percent Active Ingredient:
mL H ~SO !~normality H SO !~Factor!
2 4 2 4
g of sample
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
10.4 Active Ingredient and Factor:
listed by the American Chemical Society, see Analar Standards for Laboratory
Active Ingredient Factor
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
NH 1.703
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
NH 1.804
MD.
D5584
DETERMINATION OF QUATERNARYAMMONIUM 15.1.3 Titratewithsodiumlaurylsulfatesolutiontothecolor
COMPOUNDS IN ACQ-B SOLUTION BY TWO- change from pink to yellow-green marked by the formation of
PHASE TITRATION a white precipitate.
15.2 Add 20 mL water, 20 mL chloroform and 2 mL
11. Scope
methylene blue solution by graduated cylinder to the glass jar.
11.1 This test method is applicable to the determination of Cap the jar and shake the mixture well. Weigh3gof sample
solution (to the nearest 1 mg) into the tared jar and record the
quaternary ammonium compounds in ACQ-B working solu-
tions by titration using sodium laurylsulfate as titrant and mass. Cap the jar and shake the mixture well. Titrate with the
standardized (0.005 M) sodium laurylsulfate solution. The end
methylene blue as color indicator in a two-phase system. The
end point of the titration is indicated by a color change in the pointiswherethechloroformlayer(bottom)justbeginstoturn
blue. If the aqueous layer turns white and the chloroform layer
organic layer from colorless to light blue.
is blue then the end point has been exceeded. The detection
12. Apparatus
limit under these conditions is a solution concentration of
12.1 Microburet, 10 mL capacity graduated in 0.02 mL 0.001 % (10 ppm mass/mass) alkyl ammonium compound.
increments or digital buret, 50 mL capacity.
16. Calculation
12.2 Glass Bottles, 100 mL capacity with PTFE lined caps.
12.3 Graduated Cylinder,25mL.
16.1 M1:
12.4 Analytical Balance, 0.1 mg readability.
hyamine mass ~g!
12.5 Transfer Pipettes. hyamine solution 5
~448.1!~0.25!
12.6 Volumetric Flasks, 250 and 1000 mL.
16.2 M2:
12.7 Erlenmeyer Flasks, 125 mL.
~M1!~gof Hyamine!
12.8 Beaker, 250 mL.
sodium laurylsulfate 5
mL of sodium laurylsulfate
13. Reagents
~M2!~mL titrant!~MW of AAC!~100!
%alkyl ammonium compound 5
13.1 Sodium Laurylsulfate. ~1000!~g of sample!
13.2 Hyamine, 1622.
13.3 28,78-dichlorofluorescein. DETERMINATION OF QUATERNARYAMMONIUM
COMPOUNDS IN ACQ-B SOLUTIONS BY SINGLE-
13.4 Methylene Blue Indicator.
13.5 Sodium Sulfate. PHASE TITRATION
13.6 Sulfuric Acid, 0.43 N.
17. Scope
13.7 Chloroform.
13.8 Isopropyl Alcohol.
17.1 This test method is applicable to the determination of
didecyldimethyl ammonium chloride (DDAC) in ACQ-B
14. Solution Preparation
working solutions by titration using sodium tetraphenylboron
14.1 Sodium Laurylsulfate (0.005 M)—Dry several grams
as titrant and 28,78-dichlorofluorescein as a color indicator. For
at 105°C to constant weight. Weigh out 1.44 g of dry sodium
ACQ concentrates a suitable dilution before the analysis is
laurylsulfate (to the nearest mg) into a 250-mL beaker and
required. In the case of alkaline ACQ solutions the solution
dissolve in distilled water. Quantitatively transfer to a 1-L
shouldbefirstneutralized.Theendpointofthetitrationwillbe
volumetric flask and dilute to volume with distilled water.
indicated by a solution color change from purple-pink to
14.2 Hyamine 1622 (0.005 M)—Dry to constant weight in
lemon-green.
an oven at 100°C. Weigh 0.580 to 0.585 g (to the nearest 0.1
mg) and dissolve in distilled water. Dilute to 250 mL in a
18. Apparatus
volumetric flask.
18.1 Class A Buret,50mL.
18.2 Erlenmeyer Flask, 125 mL.
NOTE 1—Hyamine 1622 is diisobutylphenoxyethoxyethyl dimethyl
benzyl ammonium chloride.
18.3 Analytical Balance, 0.1 mg readability.
18.4 Volumetric Pipette, 5 mL.
14.3 Methylene Blue Solution—Weigh out 0.03 g of meth-
18.5 Volumetric Flask, 250 mL.
ylene blue and transfer to a 1-Lvolumetric flask. Weigh out 50
18.6 Graduated Cylinder,25mL.
g of sodium sulfate and transfer to the 1-L volumetric flask.
Dilute to volume with 0.43 N sulfuric acid.
19. Reagents
14.4 28,78-Dichlorofluorescein Color Indicator—0.1 % in
isopropyl alcohol.
19.1 Sodium Tetraphenylboron—Dissolve 0.865 g sodium
(0.0025 M) tetraphenylboron in distilled water and dilute to 1
15. Procedure
L in a volumetric flask.
15.1 Standardization of Sodium Laurylsulfate Solution: 19.2 28,78-Dichlorofluorescein, 0.1 % in isopropyl alcohol.
15.1.1 Weigh out 5 g (to the nearest 0.1 mg) Hyamine 1622 19.3 Hyamine 1622, 0.01 M—Dry Hyamine 1622 to con-
solution into a 125-mL Erlenmeyer flask. stant weight in an oven at 100°C. Weigh 1.16 to 1.17 g (to
15.1.2 Add 25 mL of distilled water and seven drops of nearest 0.1 mg) and dissolve in distilled water. Dilute to 250
2’,7’-dichlorofluorescein indicator solution. mL in a volumetric flask.
D5584
20. Standardization of Sodium Tetraphenylboron forms a more stable complex with the anionic surfactant and
Solution displaces the cationic dye from the anionic surfactant/dye
complex and from the chloroform phase. The first excess of
20.1 Pipet 5 mL of Hyamine 1622 solution into a 125-mL
Hyamine 1622 reacts with the anionic dye (erioglaucine) to
Erlenmeyer flask.
form a blue colored chloroform soluble complex.
20.2 Add 25 mL distilled water and seven drops of 28,78-
24.2 Quaternaryammoniumcompoundsarecationicsurfac-
dichlorofluorescein indi
...