European Journal of Wood and Wood Products

, Volume 70, Issue 5, pp 621–628 | Cite as

Inter-laboratory comparison of formaldehyde emission from particleboard using ASTM D 6007-02 method

  • Mohamed Z. M. SalemEmail author
  • M. Böhm
  • Š. Barcík
  • J. Srba
Originals Originalarbeiten


An inter-laboratory comparison of formaldehyde emission (FE) from laminated (PL) and uncoated (P2) particleboard (PB) with 16 mm thick-E1, used for non-structural and interior applications such as furniture materials and supplied from a commercial plant in the Czech Republic, was performed in two laboratories using the American small test chamber (ASTM D 6007-02). The results showed highly significant differences between the laboratories for PL (P<0.001), and not significant for P2 (P=0.33), and the differences between samples were significant for P2 and PL (P<0.05). The FE values ranged between 0.056 and 0.090 and from 0.088 to 0.099 ppm for PL and from 0.129 to 0.223 and from 0.175 to 0.182 ppm for P2 as measured in laboratories 1 and 2, respectively. There was a good correlation (R 2=0.84) between the formaldehyde values measured for both types of particleboards in the two laboratories. Most of the formaldehyde values were in agreement with the requirements of the California Air Resources Board (CARB) regulation. Furthermore, the results suggested that there was a higher homogeneity between the samples in laboratory 2 than in laboratory 1. The variation was related to the chamber conditions and sampling as well as inter-panel variations.


Formaldehyde Emission Formaldehyde Concentration Chamber Assembly Normal Quantile Plot Composite Wood Product 
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Vergleich der in zwei Prüfstellen gemäß ASTM D 6007-02 gemessenen Formaldehydabgabe aus Spanplatten


Die Formaldehydabgabe (FE) aus beschichteten (PL) und unbeschichteten (P2) 16 mm dicken E1-Spanplatten (PB) für nicht tragende Verwendungen im Innenbereich, wie zum Beispiel Möbel, wurde in zwei Prüfstellen verglichen. Die Platten wurden von einer Firma in Tschechien geliefert und in der kleinen Prüfkammer nach ASTM D 6007-2 geprüft. Die Ergebnisse der zwei Prüfstellen unterschieden sich bei den beschichteten Platten stark signifikant (P<0,001) und bei den unbeschichteten Platten nicht signifikant (P=0,33). Bei beiden Prüfkörpertypen P2 und PL unterschieden sich die einzelnen Proben signifikant (P<0,05). Die Werte der Formaldehydabgabe lagen in Labor 1 bei den beschichteten Platten (PL) zwischen 0,056 und 0,090 ppm und bei den unbeschichteten Platten (P2) zwischen 0,129 und 0,223 ppm. In Labor 2 wurden Werte zwischen 0,088 und 0,099 ppm für PL und für P2 zwischen 0,175 und 0,182 ppm gemessen. Die in den beiden Laboren gemessenen Formaldehydwerte beider Plattentypen korrelierten gut (R 2=0,84). Die meisten der Werte erfüllten die Anforderungen der Luftreinhaltungskommission Kaliforniens (California Air Resources Board CARB). Daneben zeigen die Ergebnisse, dass die Proben in Prüfstelle 2 homogener waren als die Proben in Prüfstelle 1. Diese Schwankung wurde auf Unterschiede zwischen den Prüfkammern, die Probennahme sowie Unterschiede zwischen den Platten zurückgeführt.

1 Introduction

Formaldehyde is now a widely present indoor air pollutant chemical that has been found at low levels in homes, offices, and the urban environment. Many consumer products including particleboards (PB) containing formaldehyde-based resins release formaldehyde vapor, leading to consumer dissatisfaction and health hazard-related complaints in the indoor air (Pickrell et al. 1986; Salthammer et al. 2010). PB is one of the major wood-based panels used in interior applications as furniture and the main source of formaldehyde emitted inside buildings causing health hazard effects.

The International Agency for Research on Cancer (IARC) conducted an evaluation of formaldehyde and concluded that there is sufficient evidence that formaldehyde is toxic and is associated with possible health hazards causing nasopharyngeal cancer in humans (i.e., in the region of the throat behind the nose). At concentrations above 0.1 ppm in air, formaldehyde can irritate the eyes and mucous membranes resulting in watery eyes. Formaldehyde inhaled at this concentration may cause headaches, a burning sensation in the throat, and difficulties breathing, as well as triggering or aggravating asthma symptoms (IARC 2004; Kim et al. 2010).

Simultaneously, good laboratory methods were of the highest importance for controlling the formaldehyde emission (FE) from exposed areas of the final product. Standard methods for measuring FE from wood based panels use test chambers. In Europe, the chamber (0.225, 1 and ≥12 m3 in volume) according to EN 717-1 (2004) and in North America the large chamber (volume ≥22 m3) according to ASTM E 1333-96 (2002) were proposed as primary reference methods. To measure the FE in a chamber takes time and requires special and expensive equipment.

Simpler laboratory methods that can be used for inhomogeneous products with good correlation to the chamber methods are therefore needed. Numerous methods have been mainly used for the determination of FE from PB and other wood products such as perforator (EN 120 1993), 24-h Japanese desiccator (JIS A1460 2001), flask (EN 717-3 1996), and Field and Laboratory Emission Cell (FLEC) (Risholm-Sundman 1999; Kim et al. 2010) methods, and good correlations have been found between the FE values of the chamber methods and those from other methods (Risholm-Sundman 1999; Sundin et al. 1987; Que et al. 2007; Que and Furuno 2007; Park et al. 2011).

However, the lack of certified reference material made it difficult to establish an inter-calibration between test methods (Bulian et al. 2003). Moreover, the significant variations in the FE measurements between laboratories were due to the heterogeneities of chamber conditions such as volume, materials, sampling air, and specific differences in test conditions, and it was reported that comparison of FE measurements carried out by different laboratories becomes important in view of their utilization for material emission databases (Wiglusz et al. 2000; Risholm-Sundman et al. 2007; Yrieix et al. 2010; Risholm-Sundman and Wallin 1999).

The California Air Resources Board (CARB) adopted a new regulation in April 2007 to reduce the FE from composite wood products (CARB 2007). The modified version of this regulation was finally approved in April 2008. This regulation proposed the reduction of FE standards from PB in two phases: Phase 1 limits the effective date to 2009 (≤0.18 ppm) and Phase 2 limits the effective date to 2010–2011 (≤0.09 ppm).

This new regulation has established the most stringent FE limits on wood products in the United States and requires that wood panels and products manufactured from wood panels be certified by a “third party” laboratory (Third Party Certifier, TPC) approved by CARB. On top of that, the secondary method, ASTM D 6007-02 (2002) which is a small-scale chamber ranging in size from 0.02 to 1 m3 with additional conditions has been specified extensively to measure the FE for the requirements of CARB and the applicable CARB limits. In this article an inter-laboratory comparison of FE measurements from PB was conducted in two different laboratories using ASTM D 6007-02 as a quality control test method.

2 Material and methods

2.1 Test material

The emission of formaldehyde was measured from freshly produced PB from a commercial plant in the Czech Republic with 16 mm thick-E1 (May, 2010) bonded with melamine–urea–formaldehyde (MUF) adhesive resin (Table 1). The boards were classified into two types; the first type from 1–5 was laminated PB (PL) and the second type from 6–10 was uncoated PB (P2). The boards were manufactured in three layers with Norway spruce (Picea abies L.) particles (17.5% of fine particles for each face and back layer with 65% of coarse particles for the core layer).
Table 1

Properties and composition of melamine–urea–formaldehyde adhesive resin

Tab. 1

Eigenschaften und Zusammensetzung des Melamin–Harnstoff–Formaldehyd-Klebstoffes



Resin content (%)b

Face: 11, Core: 7

Solid resin content (%)


Melamine content (wt % to MUF resin)

4 (in powder form)

Viscosity (mPa s at 20 °C)


pH at 20 °C



1150–1250 kg/m3

Wax (%)c


Hardener % (NH4NO3)c

3 (57% urea as solid content)

F/(M+U) molar ratio

1.1 (1.1:1)

Free formaldehyde


aLetter M represents melamine, letter U represents urea and letter F represents formaldehyde

bPercent based on oven dry weight of wood particles

cPercent based on solid content of MUF

The laminated boards were coated with melamine-impregnated decorative paper on both sides with grammage 80 g/m2. The temperature, pressure and specific press time used to manufacture the boards were 195 °C, 3.43 MPa and 14 s/mm. For the melamine-impregnated papers, alpha cellulose decorative papers were impregnated with MUF adhesives (62% solid content). The press conditions for coating the melamine-impregnated decorative papers to the PB surfaces were 180 °C press temperature, 2.6 MPa pressure and 25 s press time.

The randomly selected panels (10 panels for each type) with nominal dimensions of 2000 mm×1100 mm×16 mm, which accounted for the full number of samples, were wrapped with polyethylene film. The delivered panels were cut into test samples in order to measure the FE according to ASTM D 6007-02. Nine samples, representing randomly distributed portions of an entire panel, were tested in three groups of three (Fig. 1), resulting in three test results, which were averaged to represent one data point for the panel. The samples were edge-sealed with aluminum tape and conditioned at 23 °C ± 0.5 °C and 50% ± 5% relative humidity (RH) for 10 days prior to analysis.
Fig. 1

Schematic sampling and formaldehyde emission measurements from particleboard using small-scale chamber

Abb. 1

Versuchsdesign und Messung der Formaldehydabgabe einer Spanplatte in der kleinen Prüfkammer

2.2 Small-scale chamber (ASTM D 6007-02)

The inter-laboratory experiment was performed in a 1 m3 and 0.225 m3 small-scale chamber system in laboratory 1 (Lab1) and laboratory 2 (Lab2), respectively. The dimensions of the test samples in the chambers were as follows: 3 pieces of 220 mm × 220 mm and 3 pieces of 200 mm × 80 mm for Lab1 and Lab2, respectively. Table 2 lists the test conditions and the differences between the two chambers.
Table 2

Differences between ASTM D 6007-02 chambers and their experimental conditions

Tab. 2

Unterschiede zwischen den Prüfkammern gemäß ASTM D 6007-2 und den Versuchsbedingungen




V (m3)

Wall material

L (m2/m3)

Fan speed (m/s)

Temp. (°C)

RH (%)

N (h−1)

Q/A (m/h)



















Al: Aluminum

\(Q/A = N/L = \frac{Q/V}{A/V}\), where V: volume of closed system—the interior volume of the test chamber (m3). N: air change rate (N is equal to Q/V)—the ratio of conditioned and filtered air that enters or is replaced in the small chamber in one hour divided by the interior volume of the small chamber, air changes per hour (ACH). L: loading ratio (L is equal to A/V)—the total exposed surface area, excluding panel edges, of the product being tested divided by the test chamber’s interior volume (m2/m3). Q: make–up air flow—the quantity of conditioned and filtered air fed into the chamber per unit time (m3/h). N/L ratio: (N/L is equivalent to Q/A)—the ratio of air flow through the chamber to sample surface area (m/h)

The chamber system consisted of the chamber assembly, an air control unit, and a clean air supply system. Filtered air from a clean air supply system was adjusted to a desired temperature, RH, and an air exchange rate. The controlled air was gathered in a mixing tank which was placed in the temperature-controlled climate chamber with the chamber assembly.

The specimens were located in the chamber so that the conditioned air stream circulated all over the panel surfaces. The chamber was operated and the temperature, RH, and barometric pressure were recorded during the testing period. The chamber test was conducted at a given Q/A ratio (Table 2). The specimens remained in the operating chamber until a steady state formaldehyde concentration was reached.

2.2.1 Quantification of formaldehyde

The emission of formaldehyde was quantified according to the modified National Institute of Occupational Safety and Health (NIOSH) Test Method 3500. The method was standardized in the USA by NIOSH 3500 (1994) and has been used for the determination of formaldehyde in large-scale chambers, small-scale chambers, and when using the desiccator method.

The method is summarized as follows: air was sampled from the chamber at 0.2–1 dm3/min through two impinger bottles, the first one containing 20 ml of 1% aqueous sodium bisulfite (NaHSO3) and the second one remained empty as a blank. Portions (4 ml) of the impinger solutions were mixed with 0.1 ml of 1% chromatropic acid (1,8-dihydroxynaphthalene-3,6-disulfonic acid) solution and 6 ml concentrated H2SO4 (96%) and left for the reaction to proceed, and then cooled.

In the first step, the chromatropic acid reacts with formaldehyde to give a red–violet hydroxydiphenylmethane derivative. In the second step of the reaction, a violet quinoid oxidation product was formed with atmospheric oxygen. The concentrated sulfuric acid is a catalyst for dehydration and oxidation (Salthammer et al. 2010). Solution absorbencies were read through a UV/vis spectrophotometer set at 580 nm. The reaction is specific for formaldehyde when the pH value is <1.0. The formaldehyde concentrations are expressed in ppm.

2.3 Statistical evaluation of results

The statistical analyses of the results were carried out employing the descriptive statistical procedure, which included the calculation of means, medians, minimum and maximum values, quartiles, standard deviations (SD), standard error of mean (SEM), variance and relative coefficient of variations (CV%). The test for data normality was done using a normal quantile plot. Identification of outliers between quartiles, defined as the values exceeding 1.5 times the interval between quartiles, i.e., the interval between the 75% value and the 25% value, was also made. Moreover, analysis of variance (ANOVA) was done to investigate the significant effect of the laboratory and sample on FE values. The comparison between means was done employing a Duncan’s multiple-range test at 0.05 level of probability. Moreover, the correlation was done between the FE values resulting from the two laboratories. All analyses were performed using SAS version 8.2 (2001).

3 Results and discussion

An evaluation of the differences between the values of FE observed from the two types of PB; PL and P2 measured in two laboratories is presented in Table 3. The summary of statistics for the FE shows average values of observed parameters between both laboratories. These data are presented graphically in Figs. 24.
Fig. 2

Concentration of formaldehyde emissions from particleboard (16 mm) measured in the two laboratories

Abb. 2

In den beiden Prüfstellen gemessene Formaldehydabgabe aus den beiden Plattentypen (16 mm)

Table 3

Precision statistics for ASTM D 6007-02 results for formaldehyde emission from the two types of particleboard

Tab. 3

Ergebnisse der gemäß ASTM D 6007-2 bestimmten Formaldehydabgabe aus den zwei Spanplattentypen


Formaldehyde value (ppm)






















CV %

























Lower quartile





Upper quartile










Figure 2 shows the variation between the average of three measurements for all samples except for sample 5c, which was measured only by Lab2; the other measurement from Lab1 was not available. The relative coefficient of variation for the FE values from PL was 26.18% and 8.79%, and for P2 24.23% and 5.36%, for Lab1 and Lab2, respectively.

Furthermore, the outliers of the measured FE values presented in Fig. 3 from the two laboratories as in PL and P2 showed that there were differences between the values from the two laboratories, which indicated that Lab1 had a high number of data numerically distant from the rest of the data compared to Lab2. The normal quantile plot shown in Fig. 4 indicates that the distribution of FE values measured from Lab2 had a higher homogeneity than those from Lab1.
Fig. 3

Box–Whiskers plot of formaldehyde concentrations variation from particleboard (16 mm) between the two laboratories

Abb. 3

Unterschiede zwischen der in beiden Prüfstellen gemessenen Formaldehydabgabe aus den Spanplatten

Fig. 4

Normal quantile plot of small-scale chambers data

Abb. 4

Normal-Quantil-Plot der in den kleinen Prüfkammern gemessenen Werte

The ANOVA results in Table 4 for PL and P2, show that the differences between samples were significant for both types (P<0.05). Differences between laboratories were highly significant for PL (P<0.001) and not significant for P2 (P=0.33). However, the interactions between the samples and laboratories for the two types of PB were not significant.
Table 4

Significance levels for the effects of sample and laboratory on the overall ASTM D 6007-02 values (ppm)

Tab. 4

Signifikanzniveaus für den Einfluss der Probennahme und der Prüfstellen auf die nach ASTM D 6007-2 bestimmten Werte (ppm)


Source of variation

F value


Whole R 2

Whole CV %


Laboratory (Lab)








Lab × Sample












Lab × Sample



ns P>0.05 (not significant); * P<0.05 (significant); *** P<0.001 (highly significant)

The variability between the values of FE due to sample heterogeneity is presented in Table 5. The FE values from PL ranged between 0.056 and 0.090 and from 0.088 to 0.099 ppm for PL and from 0.129 to 0.223 and 0.175 to 0.182 ppm for P2 as measured in Lab1 and Lab2, respectively. Moreover, it was seen that the sample number 5 PL had a high amount of FE measured in both laboratories, also there were no differences between the values of FE from the PL samples measured in Lab2. On the other hand, there were differences between FE values for the same samples when measured in Lab1. In addition, the same measurement trends were found between the FE values from P2 samples measured in both laboratories, even though there were no significant differences between the two laboratories (P=0.33).
Table 5

Differences between formaldehyde emission values of two types of particleboard measured by ASTM D 6007-02 (ppm) in the two laboratories

Tab. 5

Unterschiede zwischen den Formaldehydabgabewerten der beiden Spanplattentypen, die gemäß ASTM D 6007-2 (ppm) in den beiden Prüfstellen gemessen wurden



Sample mean*




0.056±0.01 b

0.088±0.007 a

0.072±0.02 c


0.090±0.007 a

0.090±0.009 a

0.090±0.007 ab


0.062±0.02 b

0.093±0.005 a

0.078±0.02 bc


0.065±0.01 b

0.095±0.009 a

0.080±0.02 bc


0.090±0.01 a

0.099±0.01 a

0.095±0.01 a

Mean of lab*

0.072±0.02 B

0.093±0.008 A




Sample mean*




0.129±0.009 c

0.175±0.01 b

0.152±0.03 b


0.174±0.03 b

0.177±0.02 b

0.175±0.03 ab


0.163±0.05 bc

0.182±0.008 ab

0.172±0.04 ab


0.165±0.02 bc

0.182±0.007 ab

0.174±0.02 ab


0.223±0.02 a

0.181±0.009 ab

0.201±0.03 a

Mean of lab*

0.171±0.04 A

0.179±0.009 A


Values (mean ± SD). Different letters represent statistical differences between the averages of the values

*Means with the same small letter within the same column are not significantly different (P<0.05). Means with the same capital letter within the same row are not significantly different (P<0.05)

Thus, these results suggested that there was a higher homogeneity between the samples in Lab2 than in Lab1, and the most important source of variation is inter-laboratory bias due to heterogeneity of chamber conditions, and probably sampling air as well (Wiglusz et al. 2000; Risholm-Sundman et al. 2007). In addition, inter-laboratory studies provide a better understanding of the behavior measurements of the FE from the same samples of PB.

Considering that the samples received in both laboratories were distributed and selected randomly throughout the PB bundle, which makes it unlikely that the observed variations were due to inter-panel variability, there were some variations in the formaldehyde amount through the tested panel, for example; the panel PL number 1 observed differences in the samples 1a, 1b and 1c (0.065, 0.06 and 0.044 ppm, respectively as measured in Lab1) and (0.08, 0.092 and 0.093 ppm, respectively as measured in Lab2) as shown in Fig. 2. In addition, there were some variations in the average formaldehyde concentrations among the boards, (Table 5) for example the PL panels (0.056, 0.090, 0.062, 0.065 and 0.090 ppm, for panels 1, 2, 3, 4 and 5, respectively as measured in Lab1).

The obvious results of high, intermediate or low emission variations suggested that there were inter-panel variations in the formaldehyde release from PB, and these results were in agreement with previous investigations (Roffael et al. 1979).

It should be noted that the results from this inter-laboratory comparison are intended to identify TPCs that may need to work with CARB staff to enhance the precision or accuracy of their chamber testing (CARB 2010). In addition, for Lab1 which had outlier points, CARB recommends that this laboratory should calibrate its chamber as described in the recommendations of CARB, and CARB will follow up with this laboratory as necessary (CARB 2010).

Despite these differences between formaldehyde values in Lab1 and Lab2, a strongly positive acceptable linear correlation between the formaldehyde values from the two types of particleboards with 16 mm thickness had an R 2 value of 0.84 with two measurements outside the 95% confidence intervals (Fig. 5).
Fig. 5

Correlation between the formaldehyde values for 16 mm particleboards measured in the two laboratories

Abb. 5

Korrelation zwischen den in den beiden Prüfstellen gemessenen Formaldehydabgabewerten der 16 mm Spanplatten

In Fig. 3, the mean values of FE measured from PL in Lab1 (0.072 ppm) were lower than in Lab2 (0.093 ppm) and correspondingly, there were significant differences between the means, while there were no significant differences between the means of the formaldehyde emitted from P2 in Lab1 (0.171 ppm) and Lab2 (0.179 ppm).

In addition, the emission of formaldehyde from particleboards was dramatically reduced due to the lamination of the boards with melamine-impregnated paper (Fig. 3). This result was in agreement with previous results obtained in many studies relating to the effect of coating of composite wood products with different coatings like decorative vinyl film and melamine-impregnated paper on the FE values (Grigoriou 1987; Kim et al. 2010; Nemli and Öztürk 2006; Kim 2010; Salem et al. 2011).

Simultaneously, the formaldehyde concentration values from most of the PL samples measured in Lab1 and Lab2 ranged from 0.056 to 0.099 ppm, were in agreement with the CARB regulation for PB Phase 2 limit (≤0.09 ppm). Furthermore, most of the FE values from P2 ranged from 0.129 to 0.182 and these values met the requirements of the CARB Phase 1 limit (≤0.18 ppm), except for sample 10 P2 which had a high amount of formaldehyde (0.223 ppm). The CARB Phase 1 was roughly equivalent to or greater than the European E1-emission class (≤0.1 ppm), as was the Japanese F ∗∗ class (≤1.5 mg/L). Phase 2 (0.09 ppm) limits were comparable to the Japanese F ∗∗∗ limits (≈0.07 ppm), the so-called E0 levels in Europe.

4 Conclusion

The inter-laboratory results showed significant variations between the two laboratories, most of them caused by sample heterogeneity, and the inconsistency of the values was related to the chamber conditions and sampling. These results point to the necessity of having identical experimental conditions in the chambers. Moreover, there was a good correlation (R 2=0.84) between the formaldehyde values for both types of particleboards as measured according to the method of ASTM D 6007-02 in the two laboratories.

The reduction in the emission of formaldehyde from particleboards E1-16 mm measured in both laboratories resulted from coating the boards with melamine-impregnated decorative papers. Furthermore, the comparison showed that laboratory 2 gave better accuracy than laboratory 1 and suggested that laboratory 2 has sufficient experience in formaldehyde emission analysis.

As a general rule for further studies in laboratories deemed to be outliers, or whose results were identified as a concern, CARB recommends that these laboratories calibrate their small chamber in accordance with the large chamber. In this way the inter-laboratory comparisons are now very important for determination of formaldehyde emission, in addition regulations and trends need to become clearer within Central and Eastern Europe.



This work was financially supported by grants from the Internal Grant Agency, Faculty of Forestry and Wood Sciences, Czech University of Life Sciences, Prague. The authors acknowledge the contribution of the participating laboratories.


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Copyright information

© Springer-Verlag 2012

Authors and Affiliations

  • Mohamed Z. M. Salem
    • 1
    • 2
    Email author
  • M. Böhm
    • 1
  • Š. Barcík
    • 1
  • J. Srba
    • 3
  1. 1.Faculty of Forestry and Wood SciencesCzech University of Life Sciences PraguePragueCzech Republic
  2. 2.Faculty of Agriculture (EL–Shatby), Forestry and Wood Technology DepartmentAlexandria UniversityAlexandriaEgypt
  3. 3.Timber Research and Development InstitutePragueCzech Republic

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