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SeaFAST Pico-Method Guide

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0% found this document useful (0 votes)
22 views

SeaFAST Pico-Method Guide

Uploaded by

Jan Szczepaniak
Copyright
© © All Rights Reserved
Available Formats
Download as PDF, TXT or read online on Scribd
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Elemental Scientific M-SFMG-pico seaFAST-pico Method Guide

SC-DX seaFAST-pico Method Guide

SC-4 DX seaFAST pico System

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Elemental Scientific

Table of Contents

1. Introduction.........................................................................3
2. Software Configuration......................................................5
3. Offline Configuration..........................................................8
4. Inline Configuration............................................................11
5. Solution Preparation..........................................................12
6. Maintenance........................................................................12

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Elemental Scientific

1 Introduction

The seaFAST pico is a completely automated sample introduction system for determination of ultra-trace
metals in undiluted seawater. The seaFAST pico lowers procedural blanks and improves detection limits
for a variety of elements through advanced offline or online sample preparation.

seaFAST pico

■ Preconcentration mode
■ Direct mode

Diagram 1. Elements analyzed using the seaFAST pico system

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seaFAST pico Diagram
Ar
~1bar
5 4 V3P3:
Online: Nebulizer
6 Offline: Waste
3 Seawater
Preconcentraion
V3: A5e Waste Column
4mL

8 9 3 2
7 1
10 4
V1: A11b
6 10
11 5
1 11
5 9
Vacuum V2: P11 2 6
4 3 7 8
SC-DX FAST
Waste Autosampler
500µL Waste
Trace Metals
Cleanup Column

SV: V12
1 2 3
D Diluent/
Eluent

1 2 3
1 2 3

C
W
DI Water
B
1 2 3

Carrier/
Eluent

Buffer 12mL 3mL 3mL 3mL


S400V
Syringe
Pump

Di Water Buffer Carrier Diluent


Syringe Syringe Syringe Syringe © 2013 Elemental Scientific
S1 S2 S3 S4

Diagram 2. seaFAST pico System Line Assembly Diagram

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2 Software Configuration
Step 1.
Use only ESI SC version 2.8.0.114. Contact ESI if this version of software is not included with the installation materials.

Step 2.
If files have been customized in the ESI SC directory, make a backup copy of the directory. For a fresh installation, no backup is
necessary. Copy the ESI SC directory from the provided seaFAST methods folder. Paste it in the ESI folder. Merge folders and
overwrite all files.
Directory location:
Windows XP: Program Files\ESI\
Windows 7: Users\Public\ESI\

Step 3.
Make sure the autosampler and syringe unit are
powered on and communication cables are in
place.

Then, open the ESI SC software and select


Configure → Syringe.

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Elemental Scientific
Step 4.
Configure the system as follows:

Select system: S400

Sub System: S400V (seaFAST S2)

Check the box for “Enable Syringe COM”.


The syringe COM port should be detected
automatically.

Close the “Configure Syringe” window.

Step 5.
Click “Initialize.”

The software should detect and


initialize the autosampler and S400V
syringe module.

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Elemental Scientific

Step 6.
Click on the image of each rack to
choose and save desired rack type.

30 mL bottles fit in SR2-21

Step 7.
Before first use or if any valves have
been removed from the TRIO for
replacement or maintenance, click on
the FAST Control tab.

Toggle the valves between Load and


Inject multiple times to ensure the valves
are in the proper position.

If the Load and Inject lights do not


appear for any of the valves, close the
FAST Window and go to Diagnosis and
initialize the valves.

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Elemental Scientific

Step 8.
Once the solutions have been prepared
and connected to the system, select
“Prime_seaFAST” from the FAST
Sub-Method dropdown menu, and click
the Play button.

3 Offline Configuration

Step 1.
Place a 10 mL loop on valve 2, ports 7 – 10.
Step 2.
Connect valve 3, port 3 to a waste line.

Step 3.
Select Configure → prepFAST Offline

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Step 4.
a) Start with the prepFAST Offline method:
SF_pico.pof

b) Select “Enable seaFAST-pico”

c) Maintain at least 2 conditioning samples


prior to running samples. Vial 9 is configured
as a waste vial but any suitable waste vial
may be chosen.

d) Enter the sample vials and destination vials


for all samples to be processed.

e) After all sample vials and destination vials


are defined, right-click on the Method file to fill
down the entire batch.

Step 5.
To modify the loop fill time or elution parameters,
click on the method name, then right-click and
select “Set submethod Parameters.”

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Elemental Scientific

Step 6.
Factory defaults are displayed for a 50 fold
preconcentration factor (10mL to 200uL)

Using submethod parameters you can:

1) Adjust sample volume in increments of 10 mL

2) Define loop filling time for 10 mL loop. This can


be increased if more loop rinsing with sample is
desired.

3) Set the number of elution cycles for a single


destination vial. Multiple elution cycles may
enhance recovery.

4) Set the elution volume and initial flow rate for


each elution cycle. Volume should be based
upon the final, desired preconcentration factor.
(10mL / 200uL = 50x, default)

5) Set the elution final flow rate, which moves


the elution plug through the column and to the
destination vial.

Step 7.
Rename and save new prepFAST method.

Click start prepFAST to process the sample list


offline.

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4 Inline Configuration
Step 1.
Place a 4 mL loop on valve 2, ports 7 – 10.
Step 2.
Connect valve 3, port 3 to the nebulizer with a
green nebulizer line.

Step 3. Tuning the ICPMS


Go to File → Open Text File and open
SF_S2-Tune-10x.txt.

This method will provide approximately 20 minutes


of tuning signal by diluting the tuning solution by
10x. Alternate tuning files are available for shorter
tuning durations.

Ensure that “Enable FAST Control” is checked.

Close the FAST window.

Through the ICPMS software, send the


autosampler probe to a vial with tuning solution.
The seaFAST will automatically dilute the tuning
solution by 10x and introduce it into the ICPMS.

Wait approximately 60 s to begin tuning the


ICPMS.

When finished tuning, or if the tuning solution


begins to run out, send the probe to wash/rinse.
After the syringes have refilled automaticaly,
begin a new tuning injection by sending the
autosampler probe back to the tuning solution vial.

Step 4.
In the FAST window, go to File -> Open Text File
and open SF_S2-Preconcentration-Online.txt.

Ensure that “Enable FAST Control” is checked.

Close the FAST window.

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Elemental Scientific
Step 5. Start ICPMS Run
• Configure ICPMS method to acquire data for 60 – 80 s, scanning through the analytes of interest at least every 2 s.
• Set the uptake time or read delay to 230 s.
• Set the wash time to 180 s.
• Run at least two test samples. If necessary:
- Adjust the uptake time so that the elution peak appears 5-10 s after the beginning of data acquisition.
- Adjust the wash time so that all syringe actions are completed before the beginning of the following sample.
• Run at least 2 conditioning samples prior to a calibration blank or sample.

5 Solution Preparation
For the best results, all chemicals should be of the highest purity available. All containers should be acid washed and stored in a clean
environment. To prevent contamination, solutions should be prepared fresh daily. If preparing solutions in advance in larger batches,
watch the blank levels carefully in case of contamination.

Buffer:
To ~150 mL ultrapure deionized water in a clean, 500 mL bottle, add 140 mL glacial acetic acid and 140 mL 29% ammonium hydroxide
(or 148 mL of 28%; 192 mL of 22%). Dilute to approximately 500 mL. Adjust pH to 6.0 ± 0.2 by adding small amounts of either acetic
acid or ammonium hydroxide. When checking the pH, pour a small amount of buffer into a separate container so the pH probe never
comes in contact with the buffer in the bottle.

Eluent:
To ~250 mL ultrapure deionized water in a clean, 500 mL bottle, add 53 mL (80 g) nitric acid. Dilute to 500 mL.

Eluent IS:
To ~250 mL ultrapure deionized water in a clean, 500 mL bottle, add 53 mL (80 g) nitric acid and ~10 ppb of desired internal standard(s).
Dilute to 500 mL. Internal standard(s) should be suitable for preconcentration mode (see periodic table on page 3).

DI Water:
Ultrapure, deionized water

6 Maintenance
• Check the internal components of the valves every six months for signs of corrosion or wear. Replace valves, rotors, and/or stators
as necessary.
• If the system is not to be used for more than 1 week:
- Ensure that columns are conditioned. If an online or offline cycle has completed, then the columns are conditioned with buffer.
If not, ensure that the syringes are full and run the submethod “SF_Condition Columns.”
- Remove the columns and cap them with CTFE ¼-28 plugs for storage.
- Install ¼-28 unions in place of the columns.
- Place all solution lines into Eluent solution or another bottle of cleaning acid.
- Run at least one priming sequence.
- Place all solution lines into the DI water bottle.
- Run at least two priming sequences.

Elemental Scientific Phone: 1.402.991.7800 Email: [email protected]


7277 World Communications Drive Fax: 1.402.991.7799 Web: www.icpms.com
Omaha, NE 68122 USA
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