Strategically Targeted Research in Intelligent Built Environmental Systems

 

Task 1:

Experimental VOC Extraction, Material Characterization

and Full Scale Chamber Testing

 

Of

 

Thrust 1:

Material Emissions and Pollutant Transport in Building Envelopes

 

 

 

Prepared by:

 

James F Smith

Building Energy and Environmental Systems Laboratory (BEESL)

Environmental Quality Systems Center (EQS)

College of Engineering and Computer Science (ECS)

Syracuse University (SU)

149 Link Hall, Syracuse, NY 13244-1240

 

 


 


Research Objectives: The ultimate goal of this research is to develop reliable and practical integrated testing and modeling VOC methodology. This methodology will be used for rating products, and for predicting the long-term VOC concentration changes over the products’ service life.  In the future, this integrated prediction methodology will be extended to applications for other gaseous and particulate pollutants. The CHAMP model will also be useful for devising moisture control strategies that reduce risk for potential mold growth. The latter is a significant factor contributing to poor IAQ in some buildings. Future effort will also include modeling the outdoor-indoor transport of semi-volatile organics (e.g., from pesticides), particulate matter, and combustion-related gaseous such as SO2, NOx, and O3. Thus, while the significance of the current project may be broader, yet the project is currently defined and focused on specific objectives. The objectives of the present effort are:

·         Develop an extraction method to determine a total amount of VOC in the material.(subtask 1a)

·          Develop a method for material characterization that generates storage and transport coefficients for the material.(subtask 1b)

·         Develop a model for simulating the combined heat, air, moisture and pollutant (CHAMP) transport in building envelope systems, that includes VOC diffusion as well as the effects of air transport through wall cavities and cracks (task 2)

·         Benchmark the integrated approach that includes measured VOC extraction and material characterization into the prediction. Compare this prediction with data measured in a full-scale experiments on a typical wood frame wall assembly (subtask 1c).

 

Approach:

Sub Task A.

 Develop experimental technique to determine the total VOC content in the material 

 

Increasing ambient temperature and reducing total air pressure to a low vacuum level are recognized as factors that can accelerate diffusion processes. Yet the increased temperature is also recognized as a factor affecting amount of gas dissolved in the solid phase i.e., modifying the partition coefficient of VOC. Therefore, the work on development of extraction method must be performed in stages involving separately effects of increased temperature and that of vacuum.

 

Generally, to accelerate the desorption process all specimens will be subject to a mechanical extraction. The specimen will be placed in a sealed space of a grinding chamber and milled to crude powder grade (method a). The inlet of the chamber will be connected with a clean gas supply and the outlet with a sampling system that uses sorbent tubes connected in serial (for details of connection consult Figure 1).  The sorbent tubes will be analyzed by using a GC/MS.

 

 

 

 

 


                                    A.                                                                    B.

 

Figure 1. Schematic of the mechanical extraction set-ups A. 5 Stage mechanical grinding, B. Simplified Method – Ball mill grinder.

 

The  schematic – Fiqure 1 A – Is the conceptual design for a multi stage grinder that would be able to handle different kinds of materials. The staging allows the unquie abililty to test the most optim grinding size that will assist in extraction of the VOC. Air samples will be able to be taken at each stage of the grinding.

 

Fiqure 1 B. Is the design used by Little in his experiment to extract VOCs from floor tiles. The tiles were exposed to liquid nitrogen in order to freeze tile and  this made the tile brittle. The tile was inserted in the sealed  ball grinder.

The recreating this test will help expand the current knowledge base, prior to exploring other methods for extraction.

 

 

 

 

 

 

 

 

 

 

Figure 2. Schematic of the Thermal / Vacuum extraction set-ups

 

Fiqure 2 is the schematic layout of the thermal and vacuum extraction concept. The focus will look at the rapid aging by the combination of thermal and pressure to extract compounds.

 

Methods to be investigated will include:

a) Thermal extraction: The method includes both the mechanical and thermal extraction because the grinding chamber is placed in an insulated box with adjustable and controlled temperature. The temperature required for the thermal extraction will be dependent on the boiling point of the VOCs contained in the specimen. See Figure 2.

b) Vacuum extraction method: The grinding chamber will be connected to a reference chamber. Both chambers will have carefully calibrated volume and will be provided with instruments to measure and record total gas pressure. Vacuum will be applied stepwise by evacuating the reference chamber. See Figure 2.

Knowing the chamber volumes and pressure before and after opening the connecting valve one will be able to measure the pressure difference caused by the VOC diffusing out of the specimen. In case of VOC with a high molecular weight determination of the difference between expected air pressure (pressure equalization between both chambers) and the total gas pressure may be used to determine the rate of diffusion under vacuum.

 

One of the possibilities to be examined in establishing precision of the sorbent tubes is the use of a clean inert gas (nitrogen) supplied to the reference chamber to allow pressure equalization during which the VOCs will be adsorbed onto the passive sampling sorbent tubes and use them for analysis with a thermal desorber GC/MS system. After sampling and determination of the VOC extraction during this vacuum step the reference chamber is evacuated to the initial vacuum level and the next step with increased level of vacuum is executed.

 

c) Combination of methods a) and b).

 

d) Mechanical extraction, step 2. To examine effect of increased surface area of the specimen on VOC extraction the second grinding step will be applied, bringing the test material to a much finer powder.

 

e) Combination of method d) and a).

 

f) Combination of method d)  and b).

 

The methods a) through f) cover a broad range of processes involved in the VOC extraction, and will be analyzed to optimize test procedure with regard to an appropriate degree of milling, temperature, vacuum level and number of applied vacuum steps an. Figure 1 shows a bench top set up will be developed that includes air supply, a sealed chamber, specimen heating element, vacuum pump, and air sampling devices.

 

Sub Task B.

Develop an experimental procedure for material characterization

 

Material characterization is needed for defining the type of materials and their VOC adsorption, storage and removal capabilities as well as the input of material functions to the computer based models (task 2 of this thrust).

 

Material characterization may be achieved through indirect measurements such as pore-size and pore size-distribution or through direct measurements of VOC storage and transport coefficients. In the future, when appropriate correlation has been established, it is likely that either approach will be acceptable; yet, currently the characterization work must be focused on the direct measurements.

To complement the extraction procedure (subtask 1a) we are focused on a most universal and precise approach to determination of physical characteristics of VOC movement through building materials, namely a dual chamber method.

 

Figure 2 shows a schematic of the Dual Chamber system.

Figure 2 Schematic diagram of dual chamber system

 

As is shown in Figure 2, the tested material (specimen) separates two chambers. A clean air is supplied to the receiving chamber, while the air flow with constant amount of VOCs is supplied to the supply chamber. At this stage temperature in both chambers is the same but relative humidity may or may not be different (depending on the test program). Uniformity of gas concentration in each of these two chambers is ensured by a mixing fan. The average concentration of VOC in each of these two chambers is established from measurements performed of each of them.  Samples are taken from both inlet and outlet of each chamber and analyzed by GC/MS or GC/FID. When the experiment is underway, the difference between inlet and outlet of the supply chamber gives the amount of VOC entering the specimen and their average gives the mean VOC concentration. Respectively for the receiving chamber the difference gives the amount of VOC transferred through the specimen and their average givers the mean value of VOC concentration in the chamber.

 

Dual chamber method was selected to allow examining the transport of VOC through building materials between the supply and the receiving chamber under either transient or steady state solutions. This permits separating two important VOC parameters from one experiment, which are the effective diffusion and partition coefficients. Furthermore dual chamber method has better resolution for each of these parameters (Yang, 2004), which is an important aspects when developing fundamental understanding of methods for material characterization as well as input of CHAMPS models.

 

Another variant of dual chamber method will be used to examine how much valid are the current assumptions of constant effective diffusion and partition coefficients. The VOC concentration in the receiving chamber will be increased in five steps from clean air to 50% of VOC concentration in the supply chamber. To avoid distortion of flow conditions with removal of VOC by the sampling process the same amount of carrier gas and VOC will be supplied to the receiving chamber with the make-up mix. This experiment will be only conducted in a transient stage to compare with transient stage experiments where the same VOC transport was measured and averaged over a wide range of VOC concentrations.

Initially the work will be performed on single VOC and clean materials, later materials with know VOC concentration (information from Task 1a) will be used. The work will progress from a single VOC to multiple and interacting VOC mixes.

 

Sub Task C.

Conduct full-scale VOC experiments to validate the integrated testing and modeling approach

 

Figure 3 shows a schematic test of a wall assembly.

Figure 3. Schematic of test wall assembly

 

Full-scale chamber experiments will be conducted on a typical wood-framed residential wall assembly in a full-scale coupled indoor/outdoor environmental simulator (C-I/O-ES).

 

The C-I/O-ES has three major components: a 4.87 m by 3.66 m by 3.05 m high (16 ft by 12 ft by 10 ft) IEQ chamber, a 1.98 m by 3.66 m by 3.05 m high (6.5 ft by 12 ft by 10 ft) outdoor climate chamber, and a replaceable test wall assembly that separates the two test chambers.  Both chambers and their respective HVAC systems use stainless steel interior surfaces and PTFE gaskets to minimize pollutant emissions and adsorptions in the facility. The HVAC systems for the IEQ and climate chambers are both controlled with a direct digital control (DDC) system, providing accurate controls of temperature, relative humidity and pressure in both chambers.

 

The wall assembly tested is a 3.66 m ´ 3.05 m high (12 ft ´ 10 ft) section and 0.2 m (8 inches) thick. As shown in Figure 2, it is consisted of vinyl siding, water resistive barrier type P (WRB) type P (polymeric fibers) , 0.012 m (˝") oriented strand board (OSB), 0.15 m (6") mineral fiber insulation (fiberglas batt), 6 mil polyethylene vapor barrier, 0.012 m (˝") gypsum wallboard (drywall), and water-based paint.

 

A tracer gas method will be used determine the leakage flow paths. With known leakage path the characterization of flow resistance will be done with the pressure mapping. Pressure sensors will be installed across each major leakage airflow paths, and the measured pressure drop (DP) will be used in the Q = f(DP) equation to determine the airflow rate through the path. 

 

A test of VOC transport through the wall assembly under conditions of simultaneous heat, air, moisture and pollutant transport through the wall assembly will be conducted. These tests include the following conditions:

 

Test 1: Wall assembly is exposed to air pressure difference of 10 Pa (climate chamber pressurized), while 23 C and 50% RH conditions are maintained on both sides of the assembly. As the VOC initial concentration and air leakage path are known one may calculate and measure the VOC time dependent concentration in the receiving chamber (IEQ chamber).

 

Test 2: Measurements of the air leakage effect: formaldehyde and another single VOC (say, Ethyl benzene) are released at certain location(s) outside or inside of the wall. For instance one may inject known amounts of VOC to the frame wall cavity and measure VOC concentration inside the insulated cavity in the frame wall. Performing these measurements with positive, negative 10 Pa or 0 zero pressure difference permits determination of the effect of air flow on the total VOC transmission. Some of these tests will be performed over a period long enough to include not only the transient but also quasi-steady-state conditions. In such a case a constant VOC concentration will be maintained on the supply side.

 

 

Test 3: Test of mixed-convection airflow effect: as in the test 2, formaldehyde and another single VOC are released at certain location(s). This time pressure difference is 5 Pa, but the climate chamber is exposed to cold winter conditions (range of -15 to -20 C).

 

The details of test conditions will be evaluated with the simulation tool before carrying out the tests. The test scenarios may change based on the simulations to ensure the data for model validation. These test results will be analyzed and if needed one of the tests will be repeated.

Repeating the tests will require long time and application of large air pressure difference to clean the wall from the remaining concentrations from the previous test.

 

Air samples are taken from different locations of wall cavity through sample tubes installed on the wall assembly.  Air samples are also taken from both IEQ chamber and climate chamber and analyzed by GC/MS and HPLC (for “light” compounds such as formaldehyde and acetaldehyde) to determine the concentration of each VOC in both chambers.

 

Several details of these tests will be decided on the basis of computer calculations. Those details include air change rate for IEQ chamber if such is applied in addition to the measured "background leakage" and frequency of gas concentration measurements.  (Mechanical mixing will be used to uncouple the ACH from the requirement of well mixed air). Air change rate of clean air provided to both chambers will also be measured. Finally, based on measured VOC concentrations, air change rate, and surface area of the test wall assembly one may determine the rate for each VOC transport measured

 

Temperature and relative humidity (RH) are measured by thermocouples and relative humidity sensors to mapping the temperature and RH in the wall assembly, to help determine the airflow pattern in/through the wall assembly.

 

Comparison between the measured results and those predicted by the CHAMP model will be done as a benchmark validation. One should not expect the uncertainty in comparing the VOC concentration to be better than 30% of the estimated value. While the accuracy of VOC concentration measurement is within 15%, yet using Q = Q(DP) relationship from another test and only measuring DP in the actual test brings at least the same level of uncertainty. Other sources of uncertainty are effects of temperature and humidity.