Designation: D5582 − 14

Standard Test Method for

Determining Formaldehyde Levels from Wood Products
Using a Desiccator1
This standard is issued under the fixed designation D5582; 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 1.4 This standard does not purport to address all of the
1.1 This test method covers a small scale procedure for safety concerns, if any, associated with its use. It is the
measuring formaldehyde emission potential from wood prod- responsibility of the user of this standard to establish appro-
ucts under defined test conditions. The formaldehyde level is priate safety and health practices and determine the applica-
determined by collecting air-borne formaldehyde in a small bility of regulatory limitations prior to use. For specific hazard
distilled water reservoir within a closed desiccator. The quan- statements, see Section 6 and 8.2.5.
tity of formaldehyde is determined by a modification of the
National Institute for Occupational Safety and Health (NIOSH) 2. Referenced Documents
3500 chromotropic acid test procedure. Other analytical pro- 2.1 ASTM Standards:2
cedures may be used to determine formaldehyde emission E77 Test Method for Inspection and Verification of Ther-
potential provided that such methods give similar results to the mometers
chromotropic acid procedure. However, the test results and test E337 Test Method for Measuring Humidity with a Psy-
report must be properly qualified and the analytical procedure chrometer (the Measurement of Wet- and Dry-Bulb Tem-
employed must be noted. Procedures based on acetylacetone peratures)
and pararosaniline have been found to give similar results to E1333 Test Method for Determining Formaldehyde Concen-
chromotropic acid in other test methods used in determining trations in Air and Emission Rates from Wood Products
formaldehyde emission potential from wood products (see Test Using a Large Chamber
Method E1333).
2.2 HUD Document:
1.2 Wood products typically evaluated by this test method 24 CFR 3280, Manufactured Home Construction and Safety
are made with urea-formaldehyde adhesives and include Standards, Federal Register, Vol 49, No. 1553
particleboard, hardwood, plywood, and medium-density fiber- 2.3 NIOSH Document:
board. This test method is used for product quality control and Formaldehyde Method 3500, U.S. Department of Health,
is a small bench test method that correlates with the large-scale and Human Services3
acceptance test for determining formaldehyde levels from
wood products, Test Method E1333. The general desiccator 2.4 Other Documents:
testing procedure may be modified for different conditioning Minnesota Statutes Section 144.495, 325F.18, and 325F.181,
times to accommodate its use in manufacturing quality control. Formaldehyde Gases in Building Materials4
However, the test results must be properly qualified and the California Air Resources Board (CARB), California Code of
conditioning time employed must be noted. Regulations Sections 93120-93120.12, Title 17 Airborne
Toxic Control Measure to Reduce Formaldehyde Emis-
NOTE 1—If modifications are made to the conditioning period for sions from Composite Wood Products5
quality control purposes, it is important that the modification is consis-
tently applied. Otherwise, the results may not be comparable.
1.3 The values stated in SI units are to be regarded as the
2
standard. The values given in parentheses are for information For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
only. Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
3
Available from Standardization Documents Order Desk, DODSSP, Bldg. 4,
Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098, http://
1
This test method is under the jurisdiction of ASTM Committee D07 on Wood www.dodssp.daps.mil.
4
and is the direct responsibility of Subcommittee D07.03 on Panel Products. Available from Print Communications, Dept. of Administration, 117 University
Current edition approved Aug. 1, 2014. Published September 2014. Originally Ave., St. Paul, MN 55155.
5
approved in 1994. Last previous edition approved in 2006 as D5582 – 00 (2006). Available from California EPA website: http://www.arb.ca.gov/toxics/
DOI: 10.1520/D5582-14. compwood/compwood.htm.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

1
 D5582 − 14
3. Significance and Use 5.2 Petri Dish and Beaker—A clean 400-mL beaker to be
3.1 Limitations have been established on formaldehyde inverted as a reservoir support and the bottom of a 100 by
emission levels for wood panel building products made with 20-mm petri as a distilled water reservoir dish shall be
urea-formaldehyde adhesives and permanently installed in available for each desiccator test.
homes or used as components in kitchen cabinets and for 5.3 Test Room or Area—A room or test area capable of
similar industrial products. This test method is used in con- being maintained at 24 6 1°C (75 6 2°F) shall be available for
junction with the test method referenced by HUD Rules and conducting desiccator tests.
Regulations 24 CFR 3280 for manufactured housing, Califor- NOTE 3—If liquid-in-glass thermometers are used for determining or
nia Air Resources Board (CARB) regulation 93120, and by checking the temperature of the test area, see Test Method E77.
Minnesota Statutes Section 144.495 for housing units and
5.4 Examples of acceptable reagents, materials, and equip-
building materials. This test method provides a means of
ment are provided in Appendix X1.
testing small-size samples to determine formaldehyde emission
potential.
6. Hazards
3.2 This test method incorporates a desiccator, with the
6.1 Chromotropic Acid Reagent Treatment (see 8.2.4 and
desiccant removed, having a 250-mm (10-in.) inside diameter
A3.5)—During this hazardous operation, the operator shall
and a volume of approximately 10.5 L (641 in.3) with the
wear rubber gloves, apron, and a full face mask or be protected
desiccator lid in place. Conditions controlled in the procedure
from splashing by a transparent shield such as a hood window.
are as follows:
The solution becomes extremely hot during the addition of
3.2.1 Conditioning of panel products prior to testing,
sulfuric acid. Add slowly to avoid loss of sample due to
3.2.2 Specified number, size, and edge sealing of wood
splattering.
specimens to be placed in the desiccator,
3.2.3 Test desiccator temperature, and 6.2 Cleaning Chemicals for Glassware—Appropriate pre-
3.2.4 Samples from the 25-mL distilled water collection cautions shall be taken if cleaning chemicals are considered to
medium in the petri dish bottom are analyzed for formaldehyde be hazardous.
at the end of a 2-h period in the closed desiccator.
7. Test Specimens
3.3 This test method employs a single set of environmental
conditions to assess formaldehyde emission potential from 7.1 Use eight 70 6 2 mm by 127 6 2-mm (23⁄4 6 0.08 in.
certain wood products. When the relationship between desic- by 5 6 0.08 in.) by panel thickness specimens for each
cator test values and large-chamber test values are to be desiccator test. Cut specimens from the sample panel or panel
determined, the values for the specific wood panel product type segment to obtain adequate representation of areas within the
shall be plotted. This test method does allow a comparison of panel or panel segment. The fresh cut edges and ends of each
formaldehyde levels from different products for the same use. specimen shall be at least 25 mm (1 in.) from the edges and
ends of the sample panel or panel segment. When a product has
NOTE 2—Care must be exercised in the extension of the results to actual significantly different emission characteristics for each surface
formaldehyde emission from products under actual use conditions.
and has only one surface exposed to the building space, also
4. Interferences use sixteen 70 6 2 mm by 127 6 2 mm (23⁄4 6 0.08 in. by 5
6 0.08 in.) test pieces to prepare eight double-piece back-to-
4.1 The NIOSH 3500 analytical method lists phenols as a back specimens.
negative interference when present at an 8:1 excess over
formaldehyde. Modifications in the analytical procedure shall 7.2 Specimen Edge Sealing—Remove sawdust and loose
be made when this test method is used to accurately determine splinters from each test specimen. Coat the edges and ends of
the formaldehyde emission potential from wood products made each single or double-piece specimen by immersion in melted
with phenol-formaldehyde adhesive systems.6, 7 paraffin wax. Apply at least two coats. The wax shall cover no
more than 5 mm (3⁄16 in.) of either face around the coated
5. Apparatus perimeter.
5.1 Desiccator—The interior volume of the desiccator shall 7.3 Specimen Conditioning—Then condition the specimens
be 10.5 L (641 in.3). Any desiccant shall have been removed, on edge, spaced apart, so air can freely circulate across all
the interior of the desiccator thoroughly cleaned, and the surfaces for seven days 64 h at 24 6 1°C (75 6 2°F) and 50
porcelain desiccator plate replaced in the desiccator. The 6 10 % relative humidity. The formaldehyde concentration in
bearing areas of the desiccator and desiccator lid shall be the air within 30 cm (12 in.) of where the specimens are
greased so that the container will be air tight during the conditioned shall be not more than 0.04 ppm during the
duration of the 2-h test. conditioning period.
NOTE 4—Conditioning time less than seven days and specimens with
edges and ends not coated with paraffin wax may be used for quality
6
Hakes, D., Johnson, G., and Marhevka, J., Procedure for Elimination of Phenol control or informational testing; however these and other test method
Interference in the Chromotropic Acid Method for Formaldehyde, American modifications shall be clearly indicated in the test report. Modifications to
Industrial Hygiene Association, April 1984. conditioning time or edge treatment, or both, will affect the test results;
7
Technical Bulletin No. 415, National Council of the Paper Industry for Air and therefore, correlation to other test methods may need to be re-established.
Stream Improvement Inc. (NCASI), 1983. NOTE 5— If liquid-in-glass thermometers or psychrometers, or both, are

2
 D5582 − 14
used for determining or checking the temperature or the relative humidity, to drain. Do not blow out. Before placing caps on test tubes,
or both, of the conditioning area, see Test Methods E77 and E337. check the condition of the polytetrafluoroethylene (PTFE) cap
liners to make sure they are clean and not deteriorated.
8. Procedure 8.2.5 Ensure adequate mixing by use of a vibrating labora-
NOTE 6—A list of test apparatus and chemical reagents are provided in
tory mixer or other means. Mixing is complete when there is no
Appendix X1.
sign of stratification. If absorbance readings routinely exceed
8.1 Test Procedure for Materials: 1.0 or if spectrophotometric analysis is performed within 2 h,
8.1.1 Conduct tests in a room maintained at 24 6 0.6°C (75 heat capped test tubes to 95°C or place in a boiling water bath
6 1°F). Equilibrate the desiccator, petri dish bottom, and for 15 6 2 min to ensure that the chemical reaction is
distilled water to room conditions. complete. After removal, allow the test tubes to cool to room
8.1.2 Before each test, wipe the desiccator with a clean cloth temperature. Carefully vent test tubes to release pressure.
or paper towel moistened with distilled water, and then dry (Warning—Avoid rapid mixing as heating and pressure will
with a clean dry cloth or paper towel. increase and potentially break the test tube.)
NOTE 7—Formaldehyde can be used as a constituent of wet-strength 8.2.6 Allow the tubes to cool to room temperature. Do not
resins for paper and of permanent-press resins for fabrics. The type of accelerate the cooling. Avoid cooling tubes in direct sunlight as
cloth or paper towel selected for cleaning must be formaldehyde-free. this may alter color chromogen development. Transfer the
8.1.3 Apply a light coating of vacuum grease to the desic- solution to cuvettes (if necessary). At this point, small bubbles
cator lid and desiccator. Avoid excessive use of vacuum grease. may be rising through the solution. Do not make absorbance
8.1.4 Arrange specimens as prepared in 7.1 and 7.2 and readings until the solution is clear.
condition as in 7.3 on top of the porcelain desiccator plate 8.3 Absorbance Readings:
around an inverted 400-mL beaker as a 100 6 7-mm (4 6 8.3.1 Prior to performing this test method for the first time,
1⁄4-in.) high support inside the desiccator for the petri dish
a calibration curve shall be developed. See Annex A3.
bottom distilled water reservoir. Specimens should be arranged 8.3.2 Standardize the spectrophotometer using distilled wa-
so that air has access to all surfaces and edges. To obtain an ter at 580 nm in accordance with the instrument’s operating
empty desiccator reading, test one desiccator without any test instructions. The reagent blank shall be read against distilled
specimens. An empty desiccator reading greater than 0.05 water. A high absorbance for the reagent indicates contamina-
µg/mL indicates that the test system has been contaminated and tion of reagent blank or improper solution preparation. If
the test results shall be voided for all related samples in the test absorbance for the reagent blank compared to distilled water is
process. above 0.040 (using a 12-mm cell path length) or above 0.030
8.1.5 Pipet 25 mL of distilled water into the bottom portion (using a 10-mm cell path length), repeat the entire standard-
of petri dish. ization procedure.
8.1.6 Carefully lower the petri dish bottom containing 8.3.3 Zero the instrument on the reagent blank, or leave the
distilled water into the desiccator until it rests upon the inverted instrument zeroed on distilled water, and subtract the absor-
400-mL beaker. bance of the reagent blank from the absorbance of the sample
8.1.7 Slide the desiccator lid into place making sure a good solutions.
seal is obtained. 8.3.4 Read and record absorbance at 580 nm of each sample
8.1.8 Observe and record the time. prepared (see 9.1 for calculation).
8.1.9 Maintain the desiccator test room at 24 6 0.1°C (75 6 8.3.5 When a precise desiccator value is required and the
2°F). Record the temperature at 30-min intervals. Alternatively, sample solution is found to fall outside the stated absorbance
use a continuous temperature recorder. Report any temperature range (greater than 1.0 or as determined in A3.9), repeat 8.2.1
range deviations. – 8.3.4. Otherwise, report the desiccator value associated with
8.1.10 After 120 6 1 min, remove the desiccator lid and a greater than 1.0 absorbance value. When 8.2.1 – 8.3.4 are
carefully remove the petri dish. Proceed immediately to 8.2.1. repeated, appropriately dilute the sample solution to fall within
When running multiple desiccator tests, initiate 8.2.1 within 10 the preferred absorbance range of the spectrophotometer. Make
min, otherwise cover the petri dish or dishes with parafilm dilution by pipetting x mL of text solution to (4-x mL) of
while awaiting analysis. distilled water for a total of 4 mL (that is, 1 mL of test
8.2 Analysis of Water Samples: solution + 3 mL distilled water = 4 mL total). Rerunning the
8.2.1 Gently swirl the petri dish and pipet 4 mL of the distilled water “blank” is not required. Use average sample
solution into each of two 16 by 150-mm screw cap test tubes determinations as the sample absorbance. Read micrograms
for duplicate analysis. Label to avoid subsequent error. (µg) of formaldehyde from the calibration curve. (See Annex
Alternatively, use three tubes for triplicate analysis. A3.)
8.2.2 Pipet 4 mL of distilled water into a 16 by 150-mm 9. Calculation
screw capped test tube to act as a “blank.”
8.2.3 Add 0.1 mL of 1 % chromotropic acid reagent to each 9.1 Calculate formaldehyde concentration in weight per unit
test tube and shake to mix. volume in the solution from the petri dish aliquot in the
8.2.4 Slowly and carefully pipet 6.0 mL concentrated sul- desiccator:
furic acid into each test tube (Precaution—See 6.1.) and allow cs
ct 5 (1)
to flow down the side of test tube. Allow the volumetric pipet D 34

3
 D5582 − 14
where: 10.1.7 Empty desiccator reading (desiccator value of dis-
ct = µg of formaldehyde per mL of sampled solution, tilled water in desiccator containing no samples),
cs = µg of formaldehyde in 4-mL aliquot of sample read 10.1.8 If sample solution was read undiluted or diluted,
from calibration curve, and including dilution factor,
D = dilution factor, for example: 10.1.9 Desiccator value in micrograms of formaldehyde per
1 mL ~ original volume!
millilitre at test conditions; desiccator value corrected to 24°C
4 mL ~ final volume!
D 5 0.25 (2) (75°F), rounded to nearest 0.01 µg/mL,
10.1.10 Any deviations from the standard desiccator
If no dilution is made, D = 1. method shall be noted. Notations of such deviations shall
9.2 When the temperature at which the test is conducted include, but not be limited to, conditioning time, temperature
differs from 24 by 1⁄4 °C (75 by 1⁄2 °F) or more, adjust the and relative humidity during conditioning, and specimen edge
desiccator value obtained to a standard temperature of 24°C wax treatment,
(75°F) using a formula developed by Berge et al.8Annex A1 10.1.11 The analytical method employed if different from
contains a table of conversion factors for use at different the modified NIOSH 3500 chromotropic acid test procedure,
observed test temperatures as calculated using this formula. 10.1.12 Name and model number of spectrophotometer, and
The observed test temperature is the average temperature for 10.1.13 Date of test.
the total 2-h test period. 11. Precision and Bias
10. Report 11.1 Variation in the formaldehyde emission from products
evaluated by this test method is a consequence of variations in
10.1 Report the following information: the materials tested, in the conduct of the test method and the
10.1.1 Test number, analytical procedure. Limited information does exist to show
10.1.2 The manner in which samples were shipped or the variability expected between test results when the method
stored, or both: wrapped separately in vapor barrier, wrapped is used in one or more laboratories.
collectively in vapor barrier, waster sheet on top and bottom, or 11.1.1 Repeatability (Within Laboratory)—Test results indi-
with test surfaces unprotected, cate a precision of 0.06 µg/mL on the same product sample.
10.1.3 Name of product manufacturer or name of company Product manufacturing variability affects test results.9
submitting sample(s), or both, and date of manufacture, 11.1.2 Reproducibility (Between Laboratory)—A test series
10.1.4 Description of test material to include generic prod- involving five laboratories on three matched board sets from
uct name, thickness, if surface finished or sealed (both surfaces each of two products in which temperature and relative
should be described), and special treatment (if known), humidity conditioning of specimens was controlled showed an
10.1.5 Specimen conditioning details to include temperature average coefficient of variation of 15 % for products ranging in
(and range), relative humidity (and range), formaldehyde desiccator values from 0.31 to 0.69 µg/mL.9
concentration in the air, and conditioning time to nearest hour,
10.1.6 Average room temperature during the conduct of the 12. Keywords
test (see 8.1.9), 12.1 air-borne; chromotropic acid; formaldehyde levels;
small-scale; wood products

8 9
Berge, A., Mellagaard B., Hanetho, P., and Ormstad, E., Formaldehyde Release Report of Preliminary Interlaboratory Formaldehyde Large Chamber Round
from Particleboard—Evaluation of a Mathematical Model, Holz Als Roh-und Robin, Hardwood Plywood Manufacturers Association and National Particleboard
Werkstoff 38, 1980, pp. 252–255. Association, February 1987.

ANNEXES

(Mandatory Information)

A1. TEMPERATURE CONVERSION FACTORS FOR FORMALDEHYDE

A1.1 The following conversion table is based on the Berge where:

et al8 formula to correct formaldehyde concentrations for C = test formaldehyde concentration level,
temperature: Co = corrected formaldehyde concentration level,
e = natural log base,
C 5 C o ·e 2R ~ 1/t21/t o ! (A1.1)
R = coefficient of temperature (9799),
or: t = actual temperature, °K, and
C o 5 C·e R ~ 1/t21/t o ! (A1.2) to = corrected temperature, °K.

4
 D5582 − 14
TABLE A1.1 Temperature Conversion Table for Formaldehyde
9
NOTE 1—The Berge et al equation is an exponential function. The greater the variance between actual and corrected temperature, the greater the
potential error. These conversion factors shall not be applied beyond the specified test temperature range of 24 ± 1°C (75 ± 2°F).
Actual Actual
To Convert To 24°C (75°F) Multiply by To Convert To 24°C (75°F) Multiply by
°C (°F) °C (°F)
22.00 (71.6) 1.25 24.00 (75.2) 1.00
22.25 (72.1) 1.22 24.25 (75.7) 0.97
22.50 (72.5) 1.18 24.50 (76.1) 0.95
22.75 (73.0) 1.15 24.75 (76.6) 0.92
23.00 (73.4) 1.12 25.00 (77.0) 0.90
23.25 (73.9) 1.09 25.25 (77.5) 0.87
23.50 (74.3) 1.06 25.50 (77.9) 0.85
23.75 (74.8) 1.03 25.75 (78.4) 0.82
26.00 (78.8) 0.80

A2. STANDARD SOLUTIONS A AND B

A2.1 Standardization of Formaldehyde Standard Solution V = 0.100 N HCl required at pH of 9.5 from the graph
A (1.0 mg/mL) prepared in A2.1.4, mL, and
A2.1.1 Pipet 2.70 mL of 37.0 % formaldehyde solution into N = normality of HCl. The concentration of standard Solu-
a 1 L volumetric flask. Dilute to mark with freshly distilled tion A will be the average of the two analyses conducted.
water and mix well. This solution is stable for at least one A2.1.6 Record the concentration value (mg/mL) of Stan-
month in a closed container at lab conditions. dard Solution A (CA) which is the average of the two analyses
A2.1.2 Calibrate the pH meter with standard buffer solution conducted.
of pH 9.0. A2.2 Standard Solution B
A2.1.3 Pipet two 50 mL aliquots of formaldehyde standard A2.2.1 Prepare formaldehyde standard Solution B by dilut-
Solution A into two 150-mL beakers for duplicate analysis and ing 5 mL of standard Solution A to 1000 mL in a volumetric
add 20 mL of 1 M sodium sulfite (Na2SO3) to each beaker. flask using distilled water. The target concentration of Solution
Sodium sulfite solution can age, thus the 1 M sodium sulfite B is 5 µg/mL.
solution should be adjusted to 9.5 pH before adding to standard
Solution A aliquots. C B 5 ~ C A 3 1000 3 5 mL! ⁄ 1000 mL

A2.1.4 Place solution on magnetic stirrer. Immerse pH where:

electrodes into the solution and carefully titrate with 0.100 N CB = Concentration of Standard Solution B, µg/mL,
hydrochloric acid (HCl) to the original pH of the solution. CA = Concentration of Standard Solution A, mg/mL,
Record volume of HCl and corresponding pH intermittently. 1000 = Constant conversion factor,
Make a graph of pH versus volume of HCl. 5 mL = Amount of Standard Solution “A” added, and
1000 mL = Size of flask used to prepare Standard Solution
A2.1.5 Calculate the concentration, CA, of formaldehyde B.
standard Solution A in milligrams per millilitre as follows:
NOTE A2.1—This standard is stable for at least one week in a closed
V 3 N 3 30.03 ~ mg per milliequivalent! container at lab conditions.
CA 5
50 mL
A2.2.2 Record the concentration value (µg/mL) of Standard
where: Solution B (CB).

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 D5582 − 14

A3. CALIBRATION CURVE

A3.1 Prepare eight standard solutions in 200 mL volumetric 15 6 2 min to ensure that the chemical reaction is complete.
flasks by pipetting the following amounts of solution “B,” After removal, allow the test tubes to cool to room temperature.
followed by dilution to mark with distilled water.
A3.5 Standardize the spectrophotometer using distilled wa-
Target Flask
Flask # Solution “B” (mL) HCHO Concentration ter at 580 nm in accordance with the instrument’s operating
µg/mL instructions. The reagent blank (Flask #1-TT 1) shall be read
1 0.00 0.000 against distilled water. A high absorbance for the reagent
2 5.00 0.125
3 7.00 0.175 indicates contamination of reagent blank or improper solution
4 10.00 0.250 preparation. If absorbance for the reagent blank compared to
5 12.00 0.300 distilled water is above 0.040 (using a 12-mm cell path length)
6 16.00 0.400
7 20.00 0.500 or above 0.030 (using a 10-mm cell path length), repeat the
8 30.00 0.750 entire standardization procedure.
Concentration of each flask is calculated as follows:
A3.6 Zero the instrument using the reagent blank (Flask
Flask HCHO Concentration~ µ g/mL! #1-TT 1), or the instrument may be left zeroed on distilled
5 ~ C B ~ µ g/mL!! *Solution B added ~mL! / 200 mL water, and the absorbance of the reagent blank subtracted from
the absorbance of the standard solutions. Recovery shall be
A3.1.1 Record the concentration of each flask. within 65 % of reagent blank.
A3.2 Take a 4 mL aliquot from each flask specified in A3.1 A3.7 Read and record absorbance at 580 nm for each
and pipet into three test tubes for triplicate analyses. standard prepared (solutions from Flask #2-8).
A3.2.1 Note that no Solution B was added to Flask #1. Flask
#1 will be the reagent blank. A3.8 Plot absorbance against micrograms of formaldehyde
in the color developed solution. Note the amount of formalde-
Target Test Tube
Test Tube (TT) Set
HCHO Content (µg)
hyde in standard Solution Flasks, which is dependent upon the
1 0.000 standardization carried out on Standard Solution A in Annex
2 0.500 A3.
3 0.700
4 1.000 A3.8.1 The average absorbance would be plotted against the
5 1.200
6 1.600 average total micrograms of formaldehyde from each test tube
7 2.000 set.
8 3.000
A3.8.2 The absorbance of each sampled solution deter-
Test Tube HCHO Content (µg) = Flask concentration (µg/
mL) × 4. mined in 8.3.4 is compared to this calibration curve, and the
Record the content value for each test tube and that value total micrograms of formaldehyde in the aliquot is represented
will be used in step A3.8.1. as CS in 9.1.
NOTE A3.1—The calibration curve as described in this annex is
A3.3 Add 0.1 mL of 1 % chromotropic acid reagent to each provided as an example. If absorbance readings are outside of this range,
test tube. Shake tube after addition. dilute the solution with distilled water to a concentration that is within the
calibration curve. If absorbance readings exceed 1.0, place capped test
A3.4 Slowly and carefully pipet 6.0 mL concentrated sul- tubes in a boiling water bath for 15 6 2 min to ensure that the chemical
furic acid (H2SO4) into each test tube (Warning—See 7.1) and reaction is completed. Vent test tubes to release pressure. Remove tubes
allow to flow down the side of the test tube. Allow the from water bath and allow to cool to room temperature.
volumetric pipet to drain. Do not blow out. Before placing caps A3.9 Preparation of the calibration curve (A3.2 – A3.8)
on test tubes, check the condition of the polytetrafluoroethyl- shall be repeated at least once more and the final calibration
ene (PTFE) cap liners to make sure they are clean and not line shall reflect the composite of the determinations (or the
deteriorated. curve shall be calculated using a linear least squares fitting
A3.4.1 Slowly and gently agitate test tubes to affect mixing. technique). The calibration curve may not be linear at high
Mixing is complete when there is no sign of stratification. formaldehyde concentrations (high absorbance readings). If the
Carefully vent test tubes to release pressure. Rapid mixing will plot in A3.9 shows the last few points deviating from linearity,
cause heating and a pressure increase with the potential for omit the points from calculations or repeat entire procedure.
breaking the test tube. If absorbance readings exceed 1.0 or if Further, the curve should be frequently checked based on
spectrophotometric analysis is performed within 2 h, heat changes in reagent lot numbers, past experience, data
capped test tubes to 95°C or place in a boiling water bath for scattering, or instrument instability.

6
 D5582 − 14
APPENDIX

(Nonmandatory Information)

X1. REAGENTS, MATERIALS, AND EQUIPMENT FOUND SUITABLE FOR USE

X1.1 Air-Sampling Apparatus X1.2.14 Pipet, Mohr, 10 by 0.1 mL.

NOTE X1.1—Other apparatus and instruments may be used if equivalent
results are anticipated.
X1.2.15 Safety Bulb, for pipetting.
X1.1.1 Glass Desiccator, 250-mm inside diameter, total X1.2.16 Test Tubes, 16 by 150 mm, with polytetra-
volume approximately 10.5 L. fluoroethylene-(PTFE) lined screw caps.
X1.1.2 Porcelain Desiccator Plate, 230-mm diameter. X1.2.17 For repetitive analyses of sample solutions and for
added safety, use of automatic pipetting equipment may be
X1.1.3 Petri Dish, glass, bottom only, 100 by 20 mm. desirable. The following have been found suitable:
X1.1.4 Beaker, 400 mL, glass. X1.2.17.1 Brinkman Dispensers, volume 0.1 to 0.5 mL (for
chromotropic acid), volume 1 to 10 mL (for sulfuric acid), and
X1.2 Analytical Apparatus volume to 25 mL (for distilled water).
X1.2.1 Spectrophotometer.10 X1.2.17.2 Oxford Macro-Set Pipet.
X1.2.2 Spectrochek, for calibration of the spectrophotom- X1.2.17.3 Tips, 250, for transferring 4-mL aliquots.
eter. X1.2.18 Volumetric Flask, 200 mL.
X1.2.3 Beaker, 150, mL, low-form.
X1.3 Reagents
X1.2.4 Volumetric Flask, 1000 mL.
X1.3.1 Chromotropic Acid Reagent—Dissolve 0.10 g of
X1.2.5 Volumetric Flask, 100 mL. chromotropic acid (4,5-dihydroxy-2,7-naphthalene-disulfonic
X1.2.6 Volumetric Flask, two 10 mL. acid disodium salt) in freshly distilled water and dilute to 10
mL. This solution is to be made up daily.
X1.2.7 Buret, 25 mL, Class A.
X1.3.2 Sulfuric Acid, concentrated, reagent grade. Nitrate
X1.2.8 pH Meter.
concentration shall be less than 10 ppm.
X1.2.9 Magnetic Stirrer.
X1.3.3 Buffer Solution, pH 9.0.
X1.2.10 Pipet, volumetric, 4 mL.
X1.3.4 Hydrochloric Acid (HCl) 0.100 N, standard.
X1.2.11 Pipet, volumetric, 50 mL, Class A.
X1.3.5 Sodium Sulfite Solution, 1.0 M—Dissolve 12.67 g
X1.2.12 Pipet, volumetric, 6 mL, Class A. anhydrous sodium sulfite (ACS assay 99.5 %) in a 100-mL
X1.2.13 Pipet, long-tip Mohr type, 2 by 0.01 mL. volumetric flask and dilute to the mark with freshly distilled
water. The correct amount to be dissolved should be 12.6/ACS
10
assay of the anhydrous sodium sulfite actually being used (read
Milton Roy Spectronic 20 Spectrophotometer, available from scientific supply
houses, or equivalent, has been found suitable for this purpose. If you are aware of
assay from bottle label).
alternative suppliers, please provide this information to ASTM International X1.3.6 Formaldehyde Solution, 37 % W/W.
Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee,1 which you may attend. X1.3.7 Mild Liquid Soap.

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