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Volatile Organics Laboratory Analysis

Canisters must be analyzed before the sample degrades. The deadline is 30 days and begins the day the sample is taken. If samples arrive after the deadline, the cans are cleaned for reuse but are not analyzed.

The Gas Chromatograph/Ion Trap Mass Spectrometer (GC/MS) is operated in scan mode. Since this network is for long-term monitoring, the parameters are optimized for linearity and reliability and not set up for maximum sensitivity.

Calibration of the system is performed before, during and after every batch of analyses. The Mass Spectrometer tuning is checked prior to every run. Calibration samples are, at least, analyzed at the beginning, middle and end of every batch to generate the calibration curve.

The calibration consists of a 15 or 33 liter canister pressurized with CRM level certification gas cylinders. The certified standard is diluted with ultra clean zero air to reduce the 100 ppbv standard to around 5ppbv. The dilution flow is controlled by electronic flow controllers that are accurate to +/-2%. This diluted standard is compared to the NIST traceable PAMS standard. The compounds that overlap in these two standards are used to calculate the dilution ratio. This ratio is used to confirm the true amounts in the diluted standard.

A more detailed description of the analysis is available in the Standard Operating Procedures. The 44 analytes with the abbreviations, minimum detection levels, and associated Annual Guideline Concentrations (AGC's) as put forth in NYS Air Guide-1 are in Table III.

TABLE 3
Minimum Analytical Detection Limits (MDL)
Varian Saturn GC/MS with Entech model 7000 cryotrap
CHEMICAL
ABBR.
CHEMICAL MDL
ppb
AGC*
ppb
EPA
AIRS #
CAS Number
DCMA Methylene Chloride(<.3) 0.2 7.8 43802 75-09-2
CLFM Chloroform(<.2) 0.024 .009# 43803 67-66-3
12DCA 1,2 Dichloroethane(<.05) 0.03 0.01# 43815 107-06-2
111TC 1,1,1 Trichloroethane(<.2) 0.024 183 43814 71-55-6
CARBT Carbon Tetrachloride(<.2) 0.03 0.01# 43804 56-23-5
TCE Trichloroethylene(<.2) 0.025 0.08 43824 79-01-6
112TCA 1,1,2 Trichloroethane(<.1) 0.03 0.01# 43820 79-00-5
PERC Tetrachloroethylene(<1.0) 0.025 0.15 43817 127-18-4
BENZ Benzene (.05> <5.0) 0.03 0.04 45201 71-43-2
TOL Toluene (.5> <5.0) 0.035 106 45202 108-88-3
EBENZ Ethylbenzene (.05> <1.5) 0.06 230 45203 100-41-4
MPXYL M,P-Xylene (.05> <2.0) 0.06 161 45109 1330-20-7
OXYL O-Xylene (.05> <2.0) 0.04 161 45204 95-47-6
CLBEN Chlorobenzene(<.1) 0.03 23.9 45801 108-90-7
ODCBZ O-Dichlorobenzene(1,2)(<.1) 0.03 60 45805 95-50-1
MDCBZ M-Dichlorobenzene(1,3)(<.1) 0.03 60 45806 541-73-1
PDCBZ P-Dichlorobenzene(1,4)(<.5) 0.04 0.015# 45807 106-46-7
VINYL Vinyl Chloride(<.1) 0.05 0.04 43860 75-01-4
12DCP 1,2 Dichloropropane(<.2) 0.03 0.04 43829 78-87-5
124MB 1,2,4-Trimethylbenzene (.01> <1.1) 0.05 59 45208 95-63-6
135MB 1,3,5-Trimethylbenzene (.01> <.05) 0.05 59 45207 108-67-8
11DCE 1,1 Dichloroethene(<.02) 0.02 0.005# 43826 75-35-4
HCBD Hexachloro-1,3-Butadiene(<.2) 0.024 0.005# 43844 87-68-3
11DCA 1,1 Dichloroethane(<.03) 0.02 5 43813 75-34-3
CLMA Chloromethane(<2.0) 0.025 373 43801 74-87-3
CLEA Chloroethane(<2.0) 0.06 3,790 43812 75-00-3
c12CE cis 1,2-Dichloroethene(<.1) 0.03 479 43816 540-59-0
c13CP cis 1,3-Dichloropropene(<.1) 0.03 0.04 43831 542-75-6
t13CP trans 1,3-Dichloropropene(<.1) 0.04 0.04 43830 542-75-6
FR12 Dichlorodifluoromethane (.1> <2.0) 0.024 2427 43823 75-71-8
FR11 Trichlorofluoromethane (.05> <1.0) 0.03 3560 43811 75-69-4
FR113 Trichlorotrifluoroethane(<.25) 0.02 23488 43207 76-13-1
FR114 Dichlorotetrafluoroethane(<.1) 0.04 2,432 43208 76-14-2
12BEA 1,2-Dibromoethane(<.1) 0.03 0.0007# 43843 106-93-4
ACTOL A-chlorotouluene(Benzylchloride)(<.1) 0.04 0.004# 45809 100-44-7
1122C 1,1,2,2 Tetrachloroethane(<.05) 0.03 0.02 43818 79-34-5
BRMA Bromomethane(<.1) 0.03 1.29 43819 74-83-9
STYR Styrene(<1.0) 0.1 235 45220 100-42-5
BDCMA Bromodichloromethane 0.024 0.003# 43828 75-27-4
13BD 1,3 Butadiene 0.04 0.01# 43218 106-99-0
MTBE Methyl Tert Butyl Ether 0.03 834 43372 1634-04-4
2CP 2 Chloroprene 0.08 23.9 43835 126-99-8
BRFM Tribromomethane(Bromoform) 0.03 0.09 43806 75-25-2
124CB 1,2,4 Trichlorobenzene(<.3) 0.034 N/A 43810 120-82-1

# MDL is not low enough to monitor ambient air in concentration range of AGC
* Annual Guideline Concentration

The MDL, or Method Detection Limit, for this analytical procedure is calculated from 10 or more analytical runs of a standard that contains less than 0.5ppbv of each target compound. The area under the peak for each compound is imported into a spreadsheet and the standard deviation is calculated for this data set. The MDL calculation is 3 times the standard deviation (still in area counts) divided by the average area count of the 10 or more runs times the true concentration in ppbv of the standard used.

* Annual Guideline Concentration
** Minimum Detection Limit -1990-1995 (1995-1998)


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