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12

2008 vol. 1

Chemical/Petrochemical

Figure 1

Stability of sulfur compounds is

remarkable in Sulfinert®-treated cylinders.

Sulfinert

®

cylinder 3

Sulfinert

®

cylinder 2

Sulfinert

®

cylinder 1

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Hydrogen Sulfide

Carbonyl Sulfide

Methyl Mercaptan

Ethyl Mercaptan

Dimethyl Disulfide

Figure 2

Siltek® treated gas sampling cylin-

ders show very good inertness toward

mercury.

Refinery and natural gas samples often contain trace amounts of sulfur- and

mercury-containing compounds, which can interfere with reactions, poison

catalysts in petrochemical processes, and damage equipment. Because these

compounds quickly react with stainless steel surfaces, accurate determination

of these compounds is impossible when samples are collected and stored in

untreated sample cylinders. Restek’s Siltek® and Sulfinert® passivation tech-

niques bond an inert layer into the surface of stainless steel, preventing active

compounds from reacting with or adsorbing to the steel.

Accurate sulfur sampling

To characterize Sulfinert® surfaces, we tested the stability of 17ppbv standards

of sulfur compounds in three Sulfinert® sample cylinders over a 54-hour period.

Dimethyl sulfide, which is not adsorbed by stainless steel, was used as an internal

standard. The Sulfinert®-treated cylinders were inert to the reactive sulfur

compounds over the 54-hour test period (Figure 1). Hydrogen sulfide exhibited

greater than 85% recovery; methyl mercaptan, ethyl mercaptan, carbonyl sulfide,

and dimethyl disulfide exhibited greater than 90% recovery.

Sulfinert®-treated gas sampling equipment is ideal for collecting and storing

samples containing ppb levels of sulfur compounds, such as natural gas or

beverage-grade carbon dioxide. Sulfinert® treatment ensures that sulfur com-

pounds or other highly active compounds remain stable during transport

from the field to the laboratory.

Stable Mercury Results

Siltek® surface treatment has been used in a wide variety of applications in

which an inert surface is of paramount importance. To measure the impact of

Siltek® treatment on adsorption of mercury during storage, we compared the

performances of 304 grade stainless steel gas sampling cylinders (Swagelok®,

Solon OH) with and without Siltek® treatment.

We filled each cylinder with 8µg/m

3

of elemental mercury (approximately 1

part per billion) (Spectra Gases, Alpha NJ) and assessed the mercury concen-

tration in each cylinder over time to determine changes in mercury concen-

tration. Detection was achieved by direct interface gas sampling to an atomic

absorption detector. The sample pathway regulator and tubing were Siltek®

treated to ensure accurate transfer.

The data in Figure 2 demonstrate that Siltek® treatment provides a stable surface

for elemental mercury, and untreated stainless steel does not. Based on these

results, we conclude that Siltek® surface treatment for steel or stainless steel

components and tubing in CMMS and sorbent tube mercury sampling systems

will improve analytical reliability.

Siltek® and Sulfinert® surface treated cylinders and sampling components

provide an inert sample path, which prevents adsorption of active compounds

and ensures accurate sampling. For more information about these treatments,

visit us at

www.restekcoatings.com

.

Stable Sulfur &Mercury Sampling in Refineries

Using Siltek® and Sulfinert® Surface Treated Components

By Gary Barone, Restek Performance Coatings, and Irene DeGraff, Product Marketing Manager

• Reliably sample sulfur and mercury compounds at ppb levels.

• Reduce lab costs—obtain accurate results the first time.

• Detect costly process upsets, improving product yield.

Siltek

®

cylinders (n=2)

Untreated cylinders (n=2)

Acknowledgement

The authors wish to acknowledge Ted Neeme and Steve Mandel from Spectra Gases for their

contributions to this work.