ASTM D2085-89(1995)e1

Standard Test Method for Determining Chloride Used in Calculating Pentachlorophenol in Solutions or Wood (Lime Ignition Method)

SCOPE
1.1 These procedures cover the chemical analysis by the lime ignition method of treating solutions containing pentachlorophenol and of wood treated with pentachlorophenol. The method is suitable for the determination of up to 0.05 g of pentachlorophenol in treating solutions (Section 8), up to 0.05 g of pentachlorophenol in wood volumes up to 0.25 in.  (Section 9), and up to 0.25 g of pentachlorophenol in wood volumes up to 2.0 in.  (Section 11).  
1.2 This test method is not applicable to samples containing halogens other than chlorine unless appropriate correction can be made. Total halogen (excluding fluorine) is calculated as its pentachlorophenol equivalent of chloride.  
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: Historical
• Publication Date: 31-Dec-1994
• Technical Committee: D07 - Wood

Relations

• Replaced By: ASTM D2085-89(2002) - Standard Test Method for Determining Chloride Used in Calculating Pentachlorophenol in Solutions or Wood (Lime Ignition Method) (Withdrawn 2006)
• Effective Date: 27-Oct-1989

Standards Content (Sample)

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
e1
Designation: D 2085 – 89 (Reapproved 1995)
Standard Test Method for
Determining Chloride Used in Calculating
Pentachlorophenol in Solutions or Wood (Lime Ignition
Method)
This standard is issued under the fixed designation D 2085; 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.
e NOTE—Section 13 was added editorially in July 1995.
1. Scope 5. Apparatus
5.1 Crucibles, iron, nickel, or porcelain.
1.1 These procedures cover the chemical analysis by the
lime ignition method of treating solutions containing pen- 5.2 Ignition Sources:
tachlorophenol and of wood treated with pentachlorophenol. 5.2.1 Gas Burner, high-temperature of the Meker type, or
The method is suitable for the determination of up to 0.05 g of 5.2.2 Electric Muffle.
pentachlorophenol in treating solutions (Section 8), up to 0.05 5.3 Analytical Balance, sensitive to 0.001 g.
g of pentachlorophenol in wood volumes up to 0.25 in. 5.4 Magnetic Stirrer, with stirring bars (optional).
(Section 9), and up to 0.25 g of pentachlorophenol in wood 5.5 Büchner Funnel.
volumes up to 2.0 in. (Section 11). 5.6 Suction Flask.
1.2 This test method is not applicable to samples containing 5.7 Vacuum Source.
halogens other than chlorine unless appropriate correction can 5.8 Food Blender, equipped with a detachable lid and blade
be made. Total halogen (excluding fluorine) is calculated as its assembly that will fit a ⁄2-pt fruit jar threaded top (Hamilton
pentachlorophenol equivalent of chloride. Beach Model 215 or equivalent).
1.3 This standard does not purport to address all of the 5.9 Fruit Jar, ⁄2-pt, with smooth inside walls and equipped
safety concerns, if any, associated with its use. It is the with a protective cover over the assembly in case of breakage
responsibility of the user of this standard to establish appro- during blending. (Spraying the inside wall of the jar with
priate safety and health practices and determine the applica- silicone resin will prevent sticking of the lime-boring mixture.)
bility of regulatory limitations prior to use. 5.10 Miscellaneous Glassware, as required.
2. Referenced Documents 6. Reagents
2.1 ASTM Standards: 6.1 Purity of Reagents—Reagent grade chemicals shall be
D 1193 Specification for Reagent Water used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the Commit-
3. Summary of Test Method
tee on Analytical Reagents of the American Chemical Society,
3.1 An excess of silver nitrate is added to a nitric acid
where such specifications are available. Other grades may be
solution containing the chloride. The silver chloride is filtered used, provided it is first ascertained that the reagent is of
off, and the excess of silver is titrated with thiocyanate in the
sufficiently high purity to permit its use without lessening the
presence of a ferric salt. A pinkish-brown color is formed when accuracy of the determination.
excess ferric thiocyanate is produced.
6.2 Purity of Water—Unless otherwise indicated, references
to water shall be understood to mean reagent water conforming
4. Significance and Use
to Specification D 1193.
4.1 This test method covers tests for pentachlorophenol
6.3 Ammonium Thiocyanate Solution (Approximately 0.1
content in the treating solutions and the wood specimen.
N)—Dissolve 7.6 g of ammonium thiocyanate (NH CNS)
This test method is under the jurisdiction of ASTM Committee D-7 on Wood
and is the direct responsibility of Subcommittee D07.06 on Treatments for Wood “Reagent Chemicals, American Chemical Society Specifications,” Am. Chemi-
Products. cal Soc., Washington, DC. For suggestions on the testing of reagents not listed by
Current edition approved Oct. 27, 1989. Published December 1989. Originally the American Chemical Society, see “Reagent Chemicals and Standards,” by Joseph
published as D 2085 – 71. Last previous edition D 2085 – 88. Rosin, D. Van Nostrand Co., Inc., New York, NY, and the “United States
Annual Book of ASTM Standards, Vol 11.01. Pharmacopeia.”
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
e1
D 2085 – 89 (1995)
crystals containing 0.005 % or less chloride in water. Quanti- Determine the size of the sample to the nearest 0.001 g by
tatively transfer to a 1-L volumetric flask and add water exactly the weight difference in a weighing bottle containing the
to mark. Mix well. Certified, commercially prepared NH CNS
treating solution before and after sampling. Record the weight
solutions are suitable. of sample in grams as quantity A.
6.4 Calcium Hydroxide—Powdered calcium hydroxide
8.2 Cover the sample with an additional 20 g of lime-nitrate
(Ca(OH) ) containing 0.025 % or less chloride.
2 mixture and tap the crucible gently on a hard surface. Ignite the
6.5 Ferric Ammonium Sulfate Solution (Volhard Indica-
sample by either using an electric muffle or a gas burner. If an
tor)—Dissolve 10 g of ferricammonium sulfate (FeNH -
4 electric muffle is used, place the sample in the muffle and
(SO ) ·12H O) crystals containing 0.001 % or less chloride in
4 2 2 maintain at 800°C for 30 min (the muffle may be preheated if
a dilute HNO solution prepared by adding 10 mL of concen-
desired). If a gas burner is used, place the crucible on a
trated HNO to 100 mL of water.
3 supported Nichrome triangle. Light the burner and adjust the
6.6 Lime-Nitrate Mixture—Thoroughly mix 10 parts of
gas and air so that a quiet flame is obtained and small cones of
Ca(OH) with 1 part of the powdered KNO . 1 1
3 flame rise from ⁄8 to ⁄4 in. (3 to 6 mm) above the grid of the
6.7 Nitric Acid (sp gr 1.42)—Concentrated nitric acid
burner. Place the lighted burner under the supported crucible
(HNO ), containing 0.00005 % or less chloride.
3 and adjust the height of the crucible so that the distance from
6.8 Potassium Nitrate—Potassium nitrate (KNO ) crystals
3 the burner grid to the bottom of the crucible is 1 to 2 in. (25 to
containing 0.002 % or less chloride. Grind and powder the
50 mm). Heat in this position for 2 to 3 min. Readjust the
KNO using an agate or porcelain mortar and pestle or food
distance between the burner grid and the bottom of the crucible
blender sufficiently to pass through a 40-mesh screen. 1
to approximately ⁄2 in. (12 to 13 mm). Heat in this position for
6.9 Silver Nitrate, Standard Solution (0.100 N)—Dissolve
an additional 20 to 30 min. The ignited sample should be free
16.99 g of silver nitrate (AgNO ) crystals containing 0.005 %
of carbon, but no appreciable error will be introduced unless
chloride or less in water. Quantitatively transfer to a 1-L
large amounts of unburned carbon remain.
volumetric flask and add water exactly to mark. Mix well and
8.3 Cool the crucible and empty its contents into a 400-mL
store in a dark place. Certified, commercially prepared AgNO
beaker by gently tapping the crucible. Rapidly add 70 mL of
solutions are suitable.
water to the beaker and immediately place a watch glass on the
beaker. Scrub the crucible with water (or 2 % HNO if desired)
7. Standardization of NH CNS Solution
using a stirring rod equipped with a rubber policeman to loosen
7.1 Transfer 10.00 mL of 0.100 N AgNO solution to a
any remaining residue. Add the scrubbings to the beaker. The
400-mL beaker. Dilute to approximately 150 mL with water.
total aqueous volume at this point should be approximately 100
Add 5 mL of concentrated HNO and 5 mL of Volhard
mL. Place the beaker in a cold-water bath. Add 50 mL of
indicator. Titrate to a permanent (5 min or longer) pinkish- concentrated HNO either down the side of the beaker covered
brown end point with 0.1 N NH CNS solution. The NH CNS
with a watch glass or through the hole of a center hole watch
4 4
solution should be added from a buret whose smallest subdi- glass covering the beaker. Addition of HNO should be in small
visions are 0.05 mL. Estimate the amount of NH CNS solution
increments because of the vigor of the reaction. The use of an
required to the nearest 0.01 mL. Record the volume used as
acid-dispensing buret or automatic filling pipet and a magnetic
quantity E.
stirrer have been found useful in dissolving the sample. After
7.2 Calculate the equivalence factor for NH CNS, F,as the addition of HNO , the beaker may be removed from the
follows:
cold-water bath and gently heated (contents not boiled) to
promote the solution of the lime-nitrate mixture. The solution
F 5 10.00/E (1)
should be acid to Congo red paper and all lime should be in
solution. If not, add 5-mL increments of concentrated HNO
where:
until these conditions are met.
E =NH CNS solution required for the titration, mL.
8.4 Add 15.00 mL of 0.100 N AgNO solution to the beaker.
Cover with a watch glass and boil several minutes to coagulate
8. Procedure for Treating Solutions
the precipitate. Cool and filter the solution through a soft, rapid
8.1 Place 10 g of lime-nitrate mixture in a 100-mL or No. 3
paper into a 500-mL Erlenmeyer suction flask by use of an
crucible, gently tapping the crucible on a hard surface to settle
appropriately sized Büchner funnel and a vacuum source
the contents. Add the sample of treating solution (filtered if
(water aspirator source is adequate). Rinse the beaker with a
necessary) dropwise to little wells in the lime-nitrate mixture in
small quantity of water and add the rinsings to the precipitate
such a manner as to give even distribution of the sample
on the filter paper. Rinse the precipitate thoroughly with water,
without having any sample touch the sides of the crucible. The
permitting the rinsings to be added to the contents of the
sample should contain approximately 0.04 g of pentachlo-
suction flask. Test a few drops of the wash water with 0.1 N
rophenol. The sample size should approximately fit the follow-
NH CNS solution. An absence of turbidity in this test indicates
ing schedule:
that the washing is complete.
Nominal Weight % Pentachlorophenol Sample Size, g
8.5 Add 5 mL of Volhard indicator to the contents of the
2.5 1.6
suction flask. Titrate to a permanent (5 min or longer) pinkish-
5.0 0.8
7.5 0.6 brown end point with 0.1 N NH CNS. The NH CNS solution
4 4
10.0 0.4
should be added from a buret whose smallest subdivisions are
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
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e1
D 2085 – 89 (1995)
0.05 mL. Estimate the amount of NH CNS solution used to the 10.1.2 Reproducibility—Duplicate determinations on the
nearest 0.01 mL. Record the volume used as quantity B. same sample by different operators in different laboratories
8.6 Determine a correction for the pentachlorophenol carrier should not be considered suspect at the 95 % confidence level
unless it is known that the carrier is free of chloride. Follow the if they differ by 0.152 % or less.
procedures of 8.1-8.5, inclusive, except that the weight of the 10.2 Pentachlorophenol in Wood—The following criteria
sample should be approximately 2 g (determined to the nearest should be used for judging the acceptability of the results:
0.001 g). record the sample weight as A . Record the volume of 10.2.1 Repeatability—Duplicate results from runs on the
c
NH CNS solution in 8.5 as quantity B . same sample by the same operator in the same laboratory
4 c
8.7 Determine a reagent blank by following the procedures should not be considered suspect at the 95 % confidence level
of 8.1-8.5, inclusive, but using no sample. Record the volume unless they differ by more than .020 pcf.
of NH CNS solution in 8.5 as quantity B . 10.2.2 Reproducibility—Duplicate results from runs on the
4 b
8.8 Calculation: same sample by different operators in different laboratories
should not be considered suspect at the 95 % confidence level
unless they differ by more than 0.031 pcf.
P = total (uncorrected) weight percent pentachlo-
total
10.3 The foregoing precision statements are based on a
rophenol
round robin sample analysis on duplicate wood samples
= 0.5327 [(B − B)·F]/A
b c
containing about 0.35 pcf of pentachlorophenol in Southern
P = weight percent pentachlorophenol blank of
carrier
Yellow Pine sapwood as determined by six replicates of the
carrier
sample run by each of ten laboratories.
= 0.5327 [(B − B )·F]/A
b c c
10.4 These precision statements are for the test method only
P = weight percent pentachlorophenol corrected
corrected
and do not take into account the variability of treated wood in
for carrier blank
a given charge. They should not be used to measure the
=[(P − P )/(100 − P )] 3 100
total carrier carrier
reliability of operators sampling and assaying material from a
given charge or an individual piece of treated wood.
where:
A = as defined in 8.1,
3 3
11. Procedure for Wood Samples 0.25 in. (4 cm ) or Less
A = as defined in 8.7,
c
in Volume
B = as defined in 8.5,
B = as defined in 8.8,
b
NOTE 1—Samples involving wood volumes greater than 0.25 in.
B = as defined in 8.7, and
c should be subdivided into approximately equal parts and the results
F = as defined in 7.2.
averaged. Samples involving wood volumes greater than 1.0 in. are more
conveniently analyzed using the procedures of Section 10.
9. Procedure for Treating Solutions Containing More
11.1 Place 10 g of lime-nitrate mixture in a 100-mL or No.
Than 10.0 % Pentachlorophenol by Weight
3 crucible, gently tapping the crucible on a hard surface to
9.1 Weigh approximately4gof original sample into a tared settle the contents. Add the wood sample to be assayed to the
weighing bottle. Dilute with approximately four times its
surface of the lime-nitrate in such a manner that it does not
weight of heavy mineral oil and weigh again. Determine contact the edge of the crucible. Record the volume of the
weights to the nearest 0.001 g.
sample in cubic inches as quantity v.
9.2 Mix diluted solution thoroughly and transfer portions 11.2 Cover the sample with an additional 20 g of lime-
for analysis to crucible containing lime-nitrate mixture as set
nitrate mixture and tap the crucible gently on a hard surface.
forth in 8.1. Follow analytical procedures as set forth in Ignite the sample using an electric muffle or a gas burner. If an
8.2-8.7, substituting for A as follows:
electric muffle is
...