Laboratory Procedure Manual

Analyte: Selected Group of Volatile Organic

Compounds

Matrix: Air Badge

Method: GC/MS

Method No.:

Revised:

as performed by: Clayton Laboratories

Contact: Dr. Paul Epstein

1-248-344-1770

Important Information for Users

Clayton Laboratories periodically refines these laboratory methods. It is the responsibility of
the user to contact the person listed on the title page of each write-up before using the
analytical method to find out whether any changes have been made and what revisions, if
any, have been incorporated.
Volatile Organic Vapors
NHANES 1999–2000

Public Release Data Set Information

This document details the Lab Protocol for NHANES 1999–2000 data.

A tabular list of the released analytes follows:

Lab
Number Analyte SAS Label

LBXZBZ Benzene (µg/cubic meter)

LBXZCF Chloroform (µg/cubic meter)

LBXZEB Ethylbenzene (µg/cubic meter)

LBXZTE Tetrachloroethene (µg/cubic meter)

LBXZTO Toluene (µg/cubic meter)

Lab21
LBXZTI Trichloroethene (µg/cubic meter)

LBXZOX o-Xylene (µg/cubic meter)

LBXZXY m,p-Xylene (µg/cubic meter)

LBXZDB 1,4-dichlorobenzene (µg/cubic meter)

LBXZMB MTBE (µg/cubic meter)

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Volatile Organic Vapors
NHANES 1999–2000

1. SUMMARY OF TEST PRINCIPLE AND CLINICAL RELEVANCE

A selected group of volatile organic compounds in vapor form are measured by a modification of Method 7
of the Occupational Safety and Health Administration of the U. S. Dept. of Labor (OSHA). (1)The method
has been modified to use 3M 3520 Organic Vapor Monitors (OVM) (manufactured without glued-on labels)
as the sampling media and gas chromatography/mass spectrometry (GC/MS) as the detection device.(2)
Sampling times have been extended for additional sensitivity. The vapors are quantified by desorption from
the collection media with a solution of carbon disulfide and acetone, and identified and measured against a
standard curve on the GC/MS. The GC/MS is operating in the selected-ion-monitoring mode (SIM) for
additional sensitivity.

2. SAFETY PRECAUTIONS

All solvents used in this procedure are flammable. Use standard laboratory safety precautions. Carbon
disulfide is toxic and an acute fire and explosion hazard (flash point = –30°C); all work with carbon disulfide
must be performed in a hood.

3. COMPUTERIZATION; DATA SYSTEM MANAGEMENT

Raw data for all analysis is captured by the EnviroQuant software of the GC/MS instrument. Data files (raw
and processed) are stored in a directory unique to the sample and instrument on the Laboratory Information
Management System (LIMS) server. Data is backed up to tape storage each night by the Network
Administrator, and kept on the LIMS server for approximately 6 months.

When the raw and processed data has been released by the instrument analyst peer reviewer, the data is
available to the Project Manager (PM) for final calculations. Final calculations are performed by copying the
processed data into a set of Excel templates that are stored in the PM’s user directory on the laboratory’s
Novell server. Each group of samples (shipment) is stored in a separate Excel workbook. Each sample’s
data is stored on a separate tabbed page in the workbook, identified by the unique NHANES number of the
sample. The Excel templates are used to generate a comma delimited ASCII file that is transmitted
electronically to the NHANES staff when the data is released by the PM. All data for the project is stored on
the Novell server and is backed up to tape each night by the Network Administrator.

4. SPECIMEN COLLECTION, STORAGE, AND HANDLING PROCEDURES; CRITERIA FOR SPECIMEN

REJECTION

Samples are collected by the NHANES staff, sent by overnight delivery, and received at Clayton by the
sample receiving staff. The samples are taken out of the cooler and the identification marks on the samples
are compared to the paper manifest included with the samples. If the number of samples and identification
numbers match the paper manifest, the samples are logged into the Clayton LIMS. If there are
discrepancies, the PM is notified and the problems are resolved by communication with the NHANES staff.

This procedure generates a unique Clayton work order number for each shipment and a unique sample
number for each sample. These numbers have a one-to-one equivalency with the unique NHANES
shipment number and the unique individual monitor number generated by the NHANES staff, respectively.

Each sample receives a label with the numbers from the Clayton LIMS system. The group of samples from
a single shipment is placed in a plastic bag and stored in the GC/MS laboratory in refrigerator 43 or 44,
which are maintained at 4°C.

The data from an electronic manifest transmitted to the PM by NHANES is compared to the LIMS
information generated from the paper manifest. Discrepancies (if any exist) are resolved by communication
with the NHANES staff.

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Volatile Organic Vapors
NHANES 1999–2000

5. PROCEDURES FOR MICROSCOPIC EXAMINATIONS; CRITERIA FOR REJECTION OF

INADEQUATELY PREPARED SLIDES

Not applicable for this procedure.

6. EQUIPMENT AND INSTRUMENTATION, MATERIALS, REAGENT PREPARATION, CALIBRATORS

(STANDARDS), AND CONTROLS

A. Instrumentation
Hewlett Packard 5890 Series II Plus GC with cryogenic cooling capability and a Hewlett Packard 5972
MSD with EnviroQuant software.

B. Materials
Syringes:
25 mL SGE purge and trap syringe (SGE International, Part # 009462) or equivalent
SGE 007250 500 µL gas-tight syringe
SGE 006250 25 µL gas-tight syringe
SGE 009462 25 mL purge and trap syringe
Hamilton 701 10 µL syringe
Hamilton 7105NWG 5 µL syringe with Chaney adapter
SGE 031911 septum valves for syringes

Vials:
1.5 mL amber crimp seal vials – Sun International 200-002
11 mm crimp seals T/S septa – National Scientific C4011-11A
2.0 mL amber screw cap vials with T/S septa – HP 5182-0558
40 mL amber vial – VWR Scientific 15900-024
1 mL micro reaction vial – Supelco Cat. # 3-3293
15 mm Mininert valve – Supelco Cat. # 3-3301

Teflon-coated needle-nose forceps

Sonicator – Branson B-33 or equivalent
Carbon disulfide – Aldrich Cat. # 42,464-1
Acetone B&J Specto CLP grade – VWR Scientific BJ-010-1
Argon, High Purity
Argon Enclosure Hood (Custom Built) 2.5 feet × 2 feet × 2 feet (l×w×h)

C. Reagent Preparation
(1) Extraction Solvent:
The extraction solvent is prepared by mixing 2:1 v/v acetone and carbon disulfide. The mixed
solvent should be prepared fresh for each batch of samples to be extracted. The same mixed
solvent is used for preparing working standards. The sequence of steps in the preparation of the
mixed solvent for extraction (2:1 v/v acetone carbon disulfide) is as follows:

▪ 20 cc of acetone are transferred to a separate 40-mL amber vial using a syringe that is
dedicated to acetone transfer.
▪ 10 cc of carbon disulfide is withdrawn directly from the original container using a syringe
dedicated to carbon disulfide transfer. This 10-cc aliquot is then transferred to the vial
containing the acetone.

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Volatile Organic Vapors
NHANES 1999–2000

(2) Surrogate Working Solution 5000 µg/mL 4-bromofluorobenzene

A working solution of 5000 µg/mL of 4-bromofluorobenzene (BFB) is prepared by withdrawing
200 µL of a 25,000 µg/mL standard solution of BFB in methanol and transferring to a 1.5 mL clear
glass vial with a Teflon-lined septum cap. 800 µL of the acetone/carbon disulfide mixed solvent is
added. This surrogate standard should be kept refrigerated.

(3) 2:1 v/v Acetone Carbon Disulfide with Surrogate

A 30 µL aliquot of the surrogate working solutions mix is transferred to 30 mL of 2:1 acetone/CS2
mixed solvent in a vial.

D. Standards Preparation
100 µg/mL Stock Internal Standard
The stock internal standard is a solution of bromochloromethane, 1,4-difluorobenzene, and
chlorobenzene-d5 in methanol at 1000 μg/mL each (Supelco Cat. # 4-8835). A working internal
standard solution is prepared by mixing 100 µL of the stock solution with 900 µL of the 2:1
acetone/carbon disulfide mixed solvent to obtain 100 µg/mL final concentration.

External Standard Solutions

The working standard solutions are 0.1, 0.5, 2.0, 5.0, 10.0, and 20.0 (except for m-,p-xylene that do
not separate chromatographically and, therefore, are at twice the concentration and 1,3-butadiene that
is at a higher level [0.5 to 100 μg/mL]), prepared fresh for each analysis batch.

Both standards are kept in a freezer at –20°C.

Two stock standard solutions are used:

(1) a custom volatile (AccuStandard Part # S-2081-R5-10X ) mix of benzene, carbon tetrachloride,
chloroform, chloroprene, 1,4-dichlorobenzene, methylene chloride, styrene, tetrachloroethylene,
toluene, methyl tert-butyl ether, mixed xylenes, trichloroethylene, and ethylbenzene, in carbon
disulfide at a concentration of 2000 µg/mL; and

(2) 1,3-butadiene in methanol at (AccuStandard, Part # S-406A-10X) also at 2000 µg/mL.

(a) Stock 1: A stock standard of the mixed volatiles is prepared by withdrawing 100 µL of the
concentrated solution and transferring to a 1.0 mL micro-reaction vial (Supelco Cat. # 3-
3293) fitted with a Mininert valve. A 900 µL aliquot of the acetone/carbon disulfide mixed
solvent is added. This working standard is stored at –20°C when not in use, and discarded
after 1 month if not used completely.

(b) Stock 2: (10 µg/mL) a second stock standard is prepared by transferring 100 µL of Stock 1 into
a 2 mL micro-reaction vial fitted with a Mininert valve, followed by 50 µL of the concentrated
2000 µg/mL 1,3-butadiene standard, then 20 µL of 5000 µg/mL BFB, and diluted by adding
1830 µL of the 2:1 acetone/carbon disulfide mixed solvent using a 1 mL gas tight syringe. Stock
2 can be used over a 1-week period and should be stored at –20°C.

(c) Stock 2A: ( 20 µg/mL) a third stock standard is prepared by transferring 100 µL of Stock 1 into
a 2 mL micro-reaction vial fitted with a Mininert valve, followed by 50 µL of the concentrated
2000 µg/mL 1,3-butadiene standard, then 20 µL of 5000 ug/mL BFB, and diluted by adding 915
µL of the 2:1 acetone/carbon disulfide mixed solvent using a 1 mL gas-tight syringe. Stock 2
can be used over a 1-week period and should be stored at –20°C.

Working standards are prepared fresh using 1.5 mL amber autosampler vials fitted with
Teflon/silicon/Teflon septa screw tops with glass inserts. The standards are prepared one at a time
and capped immediately as follows:

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Volatile Organic Vapors
NHANES 1999–2000

▪ (0.1 µg/mL) 4 µL Stock 2 + 396 µL mixed solvent are added together in a 1 mL Mininert vial
▪ (0.5 µg/mL) 20 µL Stock 2 + 380 µL mixed solvent are added together in a 1 mL Mininert vial
▪ (2.0 µg/mL) 80 µL Stock 2 + 320 µL mixed solvent are added together in a 1 mL Mininert vial
▪ (5.0 µg/mL) 200 µL Stock 2 + 200 µL mixed solvent are added together in a 1 mL Mininert vial
▪ (10.0 µg/mL) 400 µL Stock 2 and no additional solvent in a 1 mL Mininert vial
▪ (20.0 µg/mL) 400 µL Stock 2A and no additional solvent in a 1 mL Mininert vial

E. Preparation of Quality Control Material

Quality control materials consist of unused 3M 3520 OVMs that are either fortified with the analytes of
interest, or analyzed as blank samples. The OVMs are fortified by removing the Teflon diffusion screen,
placing a piece of filter paper on the spacer plate, and injecting the appropriate amount of stock
standards to reach the concentration required. The plastic elution cap is then applied and the monitor is
allowed to sit for 16–24 hr under refrigeration. These monitors are used as Laboratory Control Samples
(LCS) or as positive controls.

7. CALIBRATION AND CALIBRATION VERIFICATION PROCEDURES

Linearity will be demonstrated by a six-point calibration curve. After the establishment of linearity (either %
relative standard deviation (RSD) <20 over working range or 0.995 correlation coefficient), a continuing
calibration check (CCC) sample is run every 10th injection. The CCC is one of the standards (usually the
middle) from the initial six-point curve.

The CCC must be within 20% agreement of the initial calibration. After each CCC and before samples are
analyzed, a laboratory solvent blank is analyzed. Calculations will be based on an average response factor,
and sample values will be corrected for extraction efficiencies.

Response factors for benzene and toluene are corrected for blank contribution. Three solvent blanks are
averaged, and the average area count is subtracted from each level of the curve. An average subtracted
response factor is generated and this response factor is used to calculate the concentration of the
contamination. This concentration is added to each level of the curve, and the corrected average response
factor is calculated.

8. PROCEDURE OPERATING INSTRUCTIONS; CALCULATIONS; INTERPRETATION OF RESULTS

A. Sample Preparation
Each charcoal pad is carefully removed from the holder and transferred to labeled vials. The vials are
labeled with the unique sample number assigned to the sample by the LIMS system. The pad is
removed using needle-nose Teflon-coated or stainless steel forceps, and is carefully folded with the aid
of a similar pair of forceps so it fits through the neck of the 1.8-mL amber vial. This procedure is carried
out in a positive pressure argon filled cabinet.

The vial is then capped and set aside in the cabinet. Once all the pads have been transferred to vials,
each vial is then reopened; one mL of the mixed solvent CS2/acetone (1:2) solution with surrogate is
added (using a dedicated gas-tight syringe) and the vial is then tightly capped and place on a holding
sample tray. When all the pads in a batch of samples to be extracted are prepared in this manner, the
tray is placed in an ultrasound bath, and enough water with a small amount of crushed ice is added to
reach the solvent meniscus but not touching the bottom of the vial caps.

The pads are then extracted by sonication for 40 minutes. Field blanks, and laboratory blanks are

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NHANES 1999–2000

similarly treated. Sample extracts are kept refrigerated in extract refrigerator 42 hr in the same vials
until they are analyzed.

B. GC/MS Settings
Typical instrument conditions are:

GC Column: Restek XTI-5 FSCC 30 m × 0.25 mm with 1-µ film thickness fused
Silica capillary column

GC Parameters: Sample Washes 1

Sample Pumps 3
Injection Volume 1.0 µL
Syringe Size 10.0 µL
Plunger Speed Fast

Temperature Program: 10°C, hold for 5 minutes, ramp at 10°C /minute to 140°C.
Injection volume = 1µL
MS Parameters:
Mode: Selected ion monitoring (SIM) injection
Splitless time 0.5 minutes.
Injection port: 200 °C
Carrier: Helium
EPC Parameters: Initial pressure 15 psi for 0.1 minutes, burst 40 psi for 0.5 minutes,
back to 15 psi, then ramp 1 psi/min to 32 psi and hold
Detector B (Transfer): 280 °C
Detector: MS Detector on 0.01 minute, MS Detector off 1.70 minute,
MS Detector on 4.76 minutes

SIM Parameters:
Group 1 Time 0.00 – 10.50 Minutes
Ions 39.0 54.0 53.0
88.0 84.0 49.0
86.0 73.0 83.0
85.0 130.0 128.0
57.0 41.0
Group 2 Time 10.50 – 114.0 Minutes
Ions 114.0 117.0 119.0
130.0 132.0 95.0
78.0 88.0 63.0
97.0

Group 3 Time 13.5 – End of Run

Ions 117.0 119.0 164.0
166.0 91.0 92.0
106.0 95.0 174.0
104.0 78.0 146.0
148.0 111.0 82.0
129.0 131.0 176.0

Mass Spec Detector Time 0.01 On

2.50 Off
6.00 On

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C. Operation
An initial curve is processed before each run of samples is processed. A run is considered a
consecutive series of sample analyses processed with no down time on the instrument of more than 24
hours. The typical run sequence consists of the:

(1) Initial six-point curve run in ascending order

(2) Several laboratory solvent blanks (3 minimum)
(3) Ten sample injections (samples include field samples, field blanks, field positive controls)
(4) Laboratory control samples (LCS, LCSD), laboratory blanks, and laboratory duplicate injections
(5) Continuing calibration check (the 2.0 µg/ml standard)
(6) Solvent blank

Repeat Steps 3, 4, 5, and 6 until all samples are analyzed

After extraction, 5 µL of the internal standard mix is transferred to an autosampler vial with glass insert
followed by 100 µL of each extract for a total volume of 105 µL. The extract vials are recapped and
stored in a refrigerator. The vials/inserts with the analytical samples are tightly capped with crimp-on
Teflon-lined septum caps and placed in the autosampler tray of the HP 5890 GC, and the analytical
sequence is started.

D. Quality Control Materials

Blank badges from the same lot as the samples and laboratory control samples (LCS) are analyzed
along with each run of samples.

E. Recording of Data
Data is recorded automatically by the EnviroQuant software of the GC/MS instrument. The data files
are sequentially numbered, and the header information fields of the files contain both the LIMS
generated sample numbers, and the NHANES transmitted identification numbers for each sample.

The data is stored on a partition of the laboratory’s NT server that is unique to each mass spectrometer
and is identified by the identification number of the mass spectrometer. For example the 2073rd data
file generated on instrument 7G would be numbered G2073 and would be stored as \\cnt-nts-
01\massspec\7g\Data\G2073.

This data is automatically backed up each night by the Network Administrator.

F. Replacement and Periodic Maintenance of Key Components

Key components for the analysis that requires routine maintenance are the column liner and septum
and the head of the GC column. Liners and septum are changed at the beginning of every analytical
sequence and the data is recorded in the laboratory notebook. Instrument flows are checked at the
same time. Other maintenance is recorded in a maintenance notebook that is kept for each instrument.

G. Preliminary Calculations
The EnviroQuant software on the GC/MS instrument identifies the compounds by retention time
windows and characteristic ions. A QUANT report is generated for each sample, along with an Internal
Standard and Surrogate Summary Report (ISSSR) for each sample. The ISSSR shows whether the
surrogate standard was within limits and whether each internal standard was within acceptance
windows. The QUANT report lists compounds identified in the sample and the amount in the injection
in nanograms.

The analyst reviews each identified compound and examines the integration performed by the
instrument. If the analyst determines that the integration was not correct, the analyst performs a
Volatile Organic Vapors
NHANES 1999–2000

manual integration on the peak of interest. The data system records the manual integration and marks
the data file as manually integrated.

The analyst also determines if the identified compound was found at a level above the linearity
determined for the system. If any compound exceeds the linearity, the analyst schedules the sample to
be reanalyzed with a dilution appropriate to bring the data within the linearity range.

The peer review analyst reviews the integrations, and initials the ISSSR along with the original analyst.
In some cases, the peer review is performed by the Project Manager at the time of final calculations.

H. Final Calculations
Final sample calculations are performed by pasting the instrument data directly into a set of Excel
templates that have been created for this project. These templates carry out the following calculations.

Front and back pads average blank loadings are subtracted from the front and back pad results
respectively. All data from blank badges run with the samples are pooled and used for background
subtraction. Data from the front sections of the badges are pooled separately from the backs and
maintained in a separate template.

Data for the front and back pads are combined according to the formula provided by the badge
manufacturer – 3M.(3) The only modification to the calculation is that the units are in nanograms not
micrograms, and the final values are in µg/m3 not mg/m3.

The formula is:

(Mass Front + 2.2 × Mass Back) × A
Conc (µg/m3) =
r × t (minutes)

Mass Front = Mass Front – Avg. Blank Mass Front

Mass Back = Mass Back – Avg. Blank Mass Back
A = Calculation Constant supplied by 3M for each analyte
r = recovery coefficient
t = sampling time (exposure) in minutes

Final reported values are recovery corrected with recovery coefficients that must be determined in
each laboratory performing the analysis according to the 3M sample guide.

9. REPORTABLE RANGE OF RESULTS

The eluted concentrations of the organic vapors are calculated from the area of the characteristic ion
measured in the sample compared to the area of the characteristic ions measured in the initial
linearity curve using an internal standard procedure. The linearity differs slightly for the different
compounds, but is linear in the range of 1–20 µg. Samples that exceed 20 µg for any component are
diluted sufficiently to be brought into the middle of the linear range, and then reanalyzed.

Elution detection limits were determined by two methods, depending on whether the compound of
interest was found to have a contribution from the blank pads. If the compound appeared in the
blank pads, the detection limit was determined to be the 99% confidence level Student-t value
times the standard deviation of the pooled blank badge data. If the compound did not appear in
the blank pads, the detection limit was determined to be the 99% confidence level Student-t value
times the standard deviation of a series of standards injected at the 1 µg level.

The reported method detection limits were calculated from the elution detection limits, the 3M
sampling rate constants, the laboratory derived desorption efficiencies, and the assumption of a
48-hour sampling period. Reported pad limits of detection are:

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Volatile Organic Vapors
NHANES 1999–2000

MDL
MDL from 3M A Pad MDL
Analyte from Std DE
blks (µg) Value µg/m3
(µg)
1,3-butadiene 0.446 0.991 23.4 3.658
2-Chloro-1,3-butadiene 0.057 0.903 31.1 0.677
Methylene chloride 1.411 1.034 26.4 12.504
Methyl tert-butyl ether 0.081 1.011 30.4 0.846
Chloroform 0.045 1.029 29.9 0.450
Carbon tetrachloride 0.085 1.082 33.1 0.900
Trichloroethene 0.038 1.118 32.2 0.383
Benzene 0.185 1.023 28.2 1.774
Tetrachloroethene 0.022 1.064 35.3 0.257
Toluene 0.399 1.156 31.8 3.808
Ethylbenzene 0.022 1.012 36. 0.277
Styrene 0.042 0.533 34.6 0.953
m-,p-xylene 0.040 1.050 36.6 0.480
o-xylene 0.030 0.890 36.6 0.434
1,4-dichlorobenzene 0.038 0.533 36.0 0.882

10. QUALITY CONTROL (QC) PROCEDURES

One LCS and one blank badge is analyzed with each run of samples. One continuing calibration verification
standard (CCV) and one solvent blank is analyzed after every ten samples. Every sample has a surrogate
standard added as part of the elution solvent.

The initial curve is considered valid if all compounds have <20% RSD over the working range. Each CCV is
considered valid if there is less than a 20% difference between the response factor calculated from the CCV
and the average response factor calculated from the initial curve.

Surrogate standards must fall within an acceptance window set from the pooled initial data sets. Surrogate
limits will be recalculated semi-annually.

Control limits have been established for the LCS samples from the initial seventeen LCS samples.

The system is declared “out-of-control” if any compound in the initial curve exceeds the 20% RSD limit. The
system is declared “out of control” if any compound in the CCV exceeds the 20% RPD limit.

Data is considered suspect if the result of any compound in the LCS exceeds the established control limits.

11. REMEDIAL ACTION IF CALIBRATION OR QC SYSTEMS FAIL TO MEET ACCEPTABLE CRITERIA

If the system is declared “out-of-control” for an initial curve, the physical system is examined to determine
the reason for the problem.

▪ The injection port on the gas chromatograph may need maintenance.

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NHANES 1999–2000

▪ The mass spectrometer source may need to be cleaned.

▪ The standards may need to be re-prepared from stocks.

No samples are run until the system is brought back into control and an initial curve passes the acceptance
criteria.

If the system is declared “out of control” for a CCV, all samples analyzed after the last acceptable CCV are
considered invalid and need to be re-analyzed. The same criteria performed for the initial curve out-of-
control are examined.

If the results for any compound in a sample exceed the highest standard in the initial curve, the extract is
diluted an appropriate amount so that it will not exceed the linearity range, and the sample is reanalyzed.
The results for the compound that exceeded linearity are calculated from the diluted injection, while the
results for the compounds that did not exceed linearity are calculated from the initial injection.

12. LIMITATIONS OF METHOD; INTERFERING SUBSTANCES AND CONDITIONS

Interfering substances are substances found in the extraction solvents or the OVM pads that are being
determined by the method. They are corrected by a blank subtraction process described in the calculation
section. Compounds with retention times and characteristic ions that are similar to the compounds of
interest can also interfere. When an interference is suspected, ratios of secondary ions can be compared to
the standards or full scan mass spectrometry can be employed to determine if an interferent is present.

If the material is present in the desorption solvent at levels comparable to the samples, it will appear at
equal levels in the front and back pad, and will be flagged as an invalid measurement because the back pad
will exceed 50% of the value of the front pad.

13. REFERENCE RANGES (NORMAL VALUES)

There are no reference ranges for this type of testing.

14. CRITICAL CALL RESULTS (PANIC VALUES)

There are no critical call results for this type of testing.

15. SPECIMEN STORAGE AND HANDLING DURING TESTING

All exposed OVMs must be kept refrigerated (4°C). Standards are kept in a freezer (–10°C). Extracts are
kept refrigerated (4°C). Badges are equilibrated to room temperature before extraction.

16. ALTERNATE METHODS FOR PERFORMING TEST OR STORING SPECIMENS IF TEST SYSTEM FAILS

There are no alternate methods of analysis for samples on OVMs. If the analytical system fails, the samples
are stored until the system is available.

17. TEST RESULT REPORTING SYSTEM; PROTOCOL FOR REPORTING CRITICAL CALLS (IF
APPLICABLE)

Sampling data is sent to the laboratory electronically by the NHANES laboratory. Sample identification
numbers, types, and sampling times are sent in a CSV data file attached to an email notification. Sample

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NHANES 1999–2000

tracking data is stored in the LIMS server.

Data is captured by the EnviroQuant software on the Hewlett-Packard Gas Chromatograph/Mass

Spectrometer system. The data is stored on the laboratory data server and processed on the PC by the
project manager. Final results are reported to NHANES by electronic transmission of a CSV formatted data
file.

Initial calibration curves are evaluated by the “Response Factor Report” generated by the EnviroQuant
system. Continuing calibration standards are evaluated by the “Evaluate Continuing Calibration Standards
Report” generated by the EnviroQuant system. Individual sample quality control data is recorded by the
EnviroQuant system on the “Internal Standard and Surrogate Summary Report”.

18. TRANSFER OR REFERRAL OF SPECIMENS; PROCEDURES FOR SPECIMEN ACCOUNTABILITY AND

TRACKING

Records of sample tracking from the LIMS server and data file captured by the EnviroQuant server are
stored on CD-ROM for archival storage. All sample identification is numeric and is not traceable in this
laboratory to any individual.

REFERENCES

1. Organic Vapors, Method 07, OSHA Sampling and Analytical Methods Manual.
2. Morandi MT, Stock TH. Personal Exposures to Toxic Air Pollutants. Vol. 2. Houston: University of
Texas; 1998.
3. Organic Vapor Monitor Sampling and Analysis Guide – Organic Vapor Monitors 3520/3530, October
1998.

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