11 calibration standards, 1 introduction, 2 standard preparation – INFICON HAPSITE Smart Plus Chemical Identification System User Manual

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HAPSITE Smart Plus Operating Manual

The SituProbe Flow Pressure method parameter should be set to supply an
excess of a few nitrogen bubbles exiting the upper holes in the purge tube
during the purge event.

Sample purge time should be set to the minimum time required to properly
purge and equilibrate the sample pathway and to collect the proper amount of
sample for concentrator methods. Experience with the analysis will determine
the correct timing.

The dry purge Nitrogen (Concentrator methods only) flow is fixed at approximately
20 mL/min, but the event time can be controlled. The amount of moisture collected
on the Concentrator during sample purging will depend on the water sample’s
temperature and the length of the ConcFill event. When moisture from the
Concentrator exits the analytical column and crosses the membrane into the mass
spectrometer, the MS pressure reading rises. Therefore, the amount of moisture
left on the Concentrator, prior to thermal desorption, must be managed to keep the
MS pressure within the software controlled limits. The proper dry purge time should
be empirically determined for the sampling conditions.

14.11 Calibration Standards

14.11.1 Introduction

Custom and ready-to-purchase calibration mixes may be purchased from a variety
of vendors. These calibration mixes are prepared in a water-soluble matrix such as
methanol for easy dilution into a known volume of water. The standard matrix must
be water soluble to evenly disperse the analytes. The low molecular weight of
methanol is below the normal scan range and therefore it is not detected by the
HAPSITE’s mass spectrometer.

14.11.2 Standard Preparation

Commercially available calibration mixes are a reliable and convenient source for
calibration standards. These standards are normally received in flame sealed glass
vials that are easily opened by snapping the flame sealed end and transferring the
contents to a screw-cap vial with a septum seal.

The water standard is prepared for immediate use by transferring a measured
quantity of the standard mix, with a syringe, into a known volume of VOC free
water. The transfer volume of the typical spiking process is a few microliters of the
standard mix into one liter of water. Two acceptable spiking techniques are:

1

Prepare the standard directly in the purging vessel. See

Figure 14-5

.

1a

Transfer a known volume of water into the purging vessel. The water level must
meet depth specifications with the probe immersed.

1b

Draw the required volume of standard mix into a syringe.

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