Horizon Technology SPE-DEX 3100 User manual

SPE-DEX®3100
Oil & Grease Extractor
Users Guide

SMARTPREP MODULE
ii
16 Northwestern Drive, Salem, NH 03079
Telephone: [phone]
Toll-Free: [phone] USA Only
Website: www.horizontechinc.com
Copyright © 2017 by Horizon Technology, Inc.
All rights reserved. Horizon Technology, Inc. reserves the right to change the infor-
mation in this document without notice. No part of this work may be processed, re-
produced, or transmitted in any form or by any means, electronic or mechanical,
including photocopying and recording, or by any information storage or retrieval sys-
tem, except as may be expressly permitted in writing by Horizon Technology, Inc.
SPE-DEX is a registered trademark of Horizon Technology, Inc.
Speed-Vap is a registered trademark of Horizon Technology, Inc.
Teflon is a registered trademark of DuPont Company.
All other product names herein are used for identification purposes only and are rec-
ognized as properties (including trademarks, registered trademarks, and referenced
copyrighted materials) of their respective holders.
P/N: 29-3100 Rev. C
(April 2017)

iii
Table of Contents
Preface..........................................................................................................................................vii
Your SPE-DEX®3100 Oil & Grease Extractor........................................................................................vii
FCC (USA).....................................................................................................................................vii
Product Safety................................................................................................................................vii
Statement of Proper Use................................................................................................................vii
Manual Audience and Intent...................................................................................................................vii
Conventions..................................................................................................................................viii
Table of Symbols ..........................................................................................................................viii
Serial Number Label .....................................................................................................................viii
Technical Support................................................................................................................................... ix
1Introduction and Safety.......................................................................................................... 1
1.1 System Overview............................................................................................................................1
1.1.1 Extractor...........................................................................................................................1
1.1.2 3100 Controller.................................................................................................................1
1.2 Product Safety Notice and Certification...........................................................................................1
1.2.1 General Safety..................................................................................................................1
1.2.2 Chemical Safety................................................................................................................2
2Theory of Operation................................................................................................................5
2.1 Oil & Grease Extraction...................................................................................................................5
2.1.1 The Goal of Oil & Grease (n-Hexane Extractable Material) Measurement.......................5
2.1.2 Methods for Oil and Grease Measurement.......................................................................5
2.1.3 The Role of Solid Phase Extraction (SPE)........................................................................6
2.1.4 Extraction Process Overview............................................................................................6
Part I: Getting Started...................................................................................................................9
3Site Preparation and Unpacking..........................................................................................11
3.1 Preparing the Site.........................................................................................................................11
3.1.1 Facility Requirements.....................................................................................................11
3.2 Unpacking the SPE-DEX 3100 Oil & Grease Extractor.................................................................12
3.3 Unpacking Checklist .....................................................................................................................15
3.3.1 3100 Controller Kit..........................................................................................................15
3.3.2 Extractor Kit....................................................................................................................15
3.3.3 Additional Requirements.................................................................................................16
3.3.4 Optional Accessories......................................................................................................17
4Overview ................................................................................................................................18
4.1 SPE-DEX 3100 Oil & Grease Extractor.........................................................................................18
4.2 SPE-DEX 3100 Controller.............................................................................................................21
5SPE-DEX 3100 System Installation .....................................................................................24
5.1 Installing the SPE-DEX 3100 System...........................................................................................24
5.1.1 Prerequisites...................................................................................................................24
5.1.2 Tools Required ...............................................................................................................24
5.1.3 System Installation Procedure........................................................................................24
5.2 Initial System Verification..............................................................................................................33
6Operation Overview ..............................................................................................................35

iv
6.1 Step 1: Conditioning......................................................................................................................36
6.2 Step 2: Load Sample ....................................................................................................................36
6.3 Step 3: Air Dry...............................................................................................................................37
6.4 Step 4: Rinse ................................................................................................................................37
7Operation Procedures ..........................................................................................................39
7.1 Setting Up for Operation ...............................................................................................................39
7.2 Loading the SPE Disk...................................................................................................................45
7.3 Running a Method.........................................................................................................................45
7.3.1 Running a Verification, Practice, or Standard Factory Method.......................................46
7.4 Running a Practice Method...........................................................................................................48
7.5 Running a Drain Function .............................................................................................................48
7.6 Running a Purge Method..............................................................................................................48
7.6.1 Purge Method Overview.................................................................................................49
7.6.2 Purge Method Sequence of Events................................................................................49
7.6.3 Procedure to Run a Purge Method.................................................................................50
7.7 Shutting Down the System............................................................................................................50
83100 Controller Features......................................................................................................52
8.1 Overview.......................................................................................................................................52
8.1.1 3100 Controller Touch Screen........................................................................................52
8.1.2 Home Page.....................................................................................................................52
8.1.3 System Page ..................................................................................................................53
8.1.4 Guide Page.....................................................................................................................53
8.1.5 Extraction Methods.........................................................................................................55
8.2 Running a Method.........................................................................................................................55
8.3 Viewing and Loading a Method.....................................................................................................56
8.3.1 Viewing a Method...........................................................................................................56
8.3.2 Loading a Method to a Station........................................................................................56
8.3.3 Loading the Same Method to All Stations.......................................................................57
8.4 Editing an Existing Method or Creating a New Method.................................................................57
8.5 Deleting a Method.........................................................................................................................61
8.6 Using Additional System Options..................................................................................................61
8.6.1 Checking Solvent Levels ................................................................................................61
8.6.2 Setting Sounds ...............................................................................................................63
8.6.3 Reviewing Raw A2D Values...........................................................................................64
8.6.4 Reviewing Statistics........................................................................................................64
8.6.5 Setting a Password.........................................................................................................65
8.6.6 Defining Sample Settings ...............................................................................................66
8.6.7 Updating Software..........................................................................................................67
8.6.8 Setting Screen Brightness..............................................................................................68
8.6.9 Performing a System Test..............................................................................................68
8.6.10 Restoring Defaults..........................................................................................................69
Part II: Maintenance and Troubleshooting...............................................................................71
9Maintenance...........................................................................................................................72
9.1 Freeing the Elute Check Valve Assembly.....................................................................................72
9.2 Cleaning the Water Sample Inlet Valve Assembly........................................................................73
9.3 Replacement of O-rings................................................................................................................74
9.4 Sample Bottle Gasket Seals .........................................................................................................74
9.5 Replacing the Disk Holder Cup O-ring..........................................................................................75

v
9.6 Assembly of the Dual Diaphragm Oil-Free Vacuum Pump ...........................................................76
9.6.1 Installing the Dual Diaphragm Oil-Free Vacuum Pump ..................................................76
9.7 Cleaning and Replacing the Elute Check Valve............................................................................77
9.7.1 Cleaning the Check Valve ..............................................................................................77
10 Troubleshooting....................................................................................................................79
10.1 Troubleshooting Tips.....................................................................................................................79
Part III: Appendices....................................................................................................................85
APreprogrammed Methods.....................................................................................................86
BParts List................................................................................................................................93
B.1 SPE Disk Holder Assemblies........................................................................................................93
B.2 SPE Disks.....................................................................................................................................93
B.3 Collection Vessels.........................................................................................................................93
B.4 Bottle Cap Adapters for the SPE-DEX3100 Extractor..................................................................94
B.5 Accessories...................................................................................................................................94
B.6 Standards and Supplies................................................................................................................94
B.7 Vacuum Requirements..................................................................................................................95
CSPE-DEX 3100 System Setup...............................................................................................97
DWarranty.................................................................................................................................99

Preface
vi

vii
Preface
Your SPE-DEX®3100 Oil & Grease Extractor
Congratulations on your purchase of the SPE-DEX 3100 Oil & Grease Extractor for hexane ex-
tractable material (HEM), the latest generation of automated Solid Phase Extraction (SPE) sys-
tems from Horizon Technology. The SPE-DEX 3100 System offers reliable automation for a
measurement that has become increasingly important over time. We are confident the SPE-DEX
3100 System will be a welcome addition to your laboratory.
FCC (USA)
The SPE-DEX 3100 Oil & Grease Extractor has been tested and found to comply with the limits
for a Class A device, pursuant to Part 15 of the FCC Rules. These limits are designed to provide
reasonable protection against harmful interferences when the equipment is operated in a commer-
cial environment. This equipment generates, uses, and can radiate radio frequency energy and, if
not installed and used in accordance with the user’s manual, may cause harmful interference to
radio communications. Operation of this equipment in a residential area is likely to cause harmful
interference in which case the user will be required to correct the interference at his/her own ex-
pense.
The SPE-DEX 3100 Oil & Grease Extractor complies with NRTL and CE certification.
Product Safety
The SPE-DEX 3100 Oil & Grease Extractor is designed with operator safety in mind. However,
the product use is at the discretion and risk of the operator or laboratory supervisor/manager. Use
the product as described in this manual, particularly referencing Section 1.2, Product Safety No-
tice and Certification.
Statement of Proper Use
The SPE-DEX 3100 Oil & Grease Extractor is a three-station extractor system designed for the
effective extraction of oil and grease from aqueous samples. It is operated by a tethered controller
and can run preprogrammed methods or methods customized by the user. The SPE-DEX 3100
System is used in conjunction with the Speed-Vap®IV for evaporation of the extracted material
to allow for gravimetric measurement.
WARNING
To reduce the risk of electrical shock, do not disassemble the SPE-DEX 3100 System. There
are no serviceable parts inside. Refer repairs to qualified service personnel.
Manual Audience and Intent
This manual, which is intended for all SPE-DEX 3100 Oil & Grease Extractor users in the la-
boratory environment, provides the information needed to operate and maintain the SPE-DEX
3100 System. The information may contain typographical errors or technical inaccuracies and is
subject to change without notice. Modifications or enhancements may also be made to the prod-
uct at any time. For the most current information, consult the Horizon Technology website at:
www.horizontechinc.com.

Preface
viii
Conventions
The following table provides examples of conventions used in Horizon Technology manuals.
Example
Description
Declaration of Conformity
Italicized text indicates document and section titles as well as
special notes.
Setup.Exe
Courier type indicates a program file name.
OK/Save as
Bold type indicates a button or information displayed on the
screen.
WARNING Symbols to the left of WARNING, CAUTION, or NOTE in-
dicate the type of danger that could be present, such as high
voltage, fire, explosion, etc. See the Table of Symbols, below,
for details.
Table of Symbols
The following symbols point out important information and alert you to potential hazards.
Symbol
Type
Description
Warning
A potentially hazardous situation, which if not avoided could result in
death or serious injury.
Note A safety note for operation or additional explanation. This informs and
guides you in safe practices to avoid injury and is intended to cover gen-
eral safety requirements for a laboratory. Each laboratory is responsible
for implementing and communicating its unique safety requirements and
program to all workers.
Caution
A caution concerning potential eye injury. Eye protection in the form of
safety glasses or goggles is highly recommended when operating the
SPE-DEX 3100 Module and any chemical processing. If reagents, liq-
uids, or vapors come into contact with the eyes, follow the appropriate
first aid procedures set forth in the laboratory’s safety manual.
Caution A caution concerning the potential of a fire.
Caution A caution to wear protective gloves when handling harmful reagents.
Serial Number Label
The following is a sample of the serial number label located on the back of the SPE-DEX 3100
Oil & Grease Extractor.

Technical Support
ix
The following is an example of the serial number located on the underside of the SPE-DEX 3100
Controller.
Technical Support
Visit the Horizon Technology website for technical information in addition to that provided in
this manual: www.horizontechinc.com. If you have questions about the SPE-DEX 3100 Oil &
Grease Extractor that are not fully addressed in this manual or our website, please contact the
Horizon Technology Technical Customer Support Center:
Phone: [phone]
Fax: [phone]
E-mail: [e-mail]
Customer Support Center hours are Monday through Friday, 8:00 a.m. to 5:00 p.m. EST. The
Center provides expert technical support including troubleshooting, repair instructions, service
and installation scheduling, and replacement part information.
15-19##
SPE-DEX® 3100 Extractor System
13.8 VDC, 1.5 A from Controller
USA Patents 5,753,105 6,027,638
Other patents pending
16 Northwestern Drive, Salem, NH 03079
SPE-DEX® 3100 Extractor Controller
15 VDC, 1.5 A
16 Northwestern Drive, Salem, NH 03079
153535200027

Preface
x
Notes:

1
1 Introduction and Safety
1.1 System Overview
The SPE-DEX 3100 System is designed to handle the extraction of oil and grease/n-hexane ex-
tractable material from aqueous samples. Capable of using 47 mm and 100-mm Solid Phase Ex-
traction (SPE) disks, the easy-to-use workstation sets new standards for both the speed of sample
extraction and the reproducibility of results.
The SPE-DEX3100 Oil & Grease Extractor enables testing facilities (laboratories) to:
•Reduce laboratory costs
•Reduce manpower requirements for testing
•Provide more reliable results by reducing testing variability
•Improve operator safety by reducing exposure to solvents
•Provide an increased level of productivity to the laboratory
The SPE-DEX 3100 System consists of two main components: the Extractor and Controller.
1.1.1 Extractor
The SPE-DEX 3100 Oil & Grease Extractor is a fully automated extraction system, which con-
sists of three extractor stations. The operator simply loads the SPE disk, a collection vessel, and
the water sample. The System automatically introduces all necessary solvents, filters the water
sample, rinses the sample bottle, and then extracts the oil and grease from the disk. The solvent
vapor exhaust fan allows bench top operation when connected to an exhaust system or operated
under a fume hood.
Specification
Description
Dimensions
18.7” W x 18.6” D x 21.5” H (47.5 x 47.2 x 54.6 cm)
Weight
58 lbs (26.3 kg)
Power 13.8 VDC (from controller)
1.1.2 3100 Controller
The SPE-DEX 3100 Controller provides operating power and programming logic for three ex-
tractor stations. The 3100 Controller is preprogrammed with a variety of optimized methods to
handle a full range of oil and grease samples and disk configurations. You can use these factory-
preset methods, or create and modify up more than thirty (30) new methods. Creating custom
methods enables you to optimize the operating parameters to meet your unique requirements
and/or take advantage of new SPE disk technology as it becomes available.
Specification
Description
Dimensions 9” W x 6.5” D x 3” H (22.9 x 16.5 x 7.6 cm)
Weight
1.7 lbs (0.771 kg)
Power
120-240 VAC/15 VDC operating, 1.5 A
1.2 Product Safety Notice and Certification
1.2.1 General Safety

1: Introduction and Safety
2
•Eye protection in the form of safety glasses or goggles is highly recommended when operating
the SPE-DEX 3100 Oil & Grease Extractor or any chemical processing. If reagents, liquids, or
vapors come into contact with the eyes, follow the appropriate first aid procedures set forth in
the laboratory’s safety manual.
•Lab coats should be provided for protection. They should be worn at all times when operating
the SPE-DEX 3100 Oil & Grease Extractor.
•Protection of the hands is essential when working with reagents or any hazardous material.
Wear gloves selected on the basis of the hazard. If reagents or other chemicals come into con-
tact with the skin, follow the appropriate first aid procedures set forth in the laboratory’s safe-
ty manual.
•The SPE-DEX 3100 Oil & Grease Extractor is designed for bench top or fume hood operation.
If installed on a bench top, the reagent bottles could be placed under a vapor vent exhaust fan.
The end of the exhaust hose should be ducted into a local exhaust device to avoid the dis-
charge of potentially toxic vapors and fumes into the laboratory atmosphere. The equipment
must be set up and operated in a well-ventilated area.
•Do not work with volatile reagents without adequate ventilation from chemical fume hoods or
other protective devices.
•The SPE-DEX 3100 Oil & Grease Extractor is designed to use only n-hexane, petroleum
ether, and methanol on a regular basis. Acetone is recommended as a cleanup step for the in-
ternal waste lines; however, it should be immediately followed by a water rinse to limit its
contact time with internal components. The use of acetone in any way other than described, or
the use of any other solvent, will compromise critical valve seals and components and void all
warranties.
•The only solvent containers that should be used with the SPE-DEX 3100 Oil & Grease Extrac-
tor are the 5-L stainless steel Solvent Delivery Systems provided with the system. The solvent
canisters are pressurized to deliver solvent to the extractor units. The use of any other contain-
ers may lead to structural failure resulting in personal injury.
•The only wastewater recovery container that should be used with the SPE-DEX 3100 Oil &
Grease Extractor is the 20-liter water waste recovery bottle (P/N 50-1686-00). High vacuum is
pulled on the recovery bottle; the use of any other bottle may lead to structural failure result-
ing in personal injury.
•During the purge and rinse cycle, solvent is sprayed from the opening on the water inlet valve.
Be sure a sample bottle is in position before pressing PURGE or START to avoid solvent being
sprayed into the atmosphere and possibly causing injury to laboratory workers.
•The Solvent Delivery System canister must be properly grounded for safe operation. Follow
the installation instructions carefully.
1.2.2 Chemical Safety
•A Material Safety Data Sheet (MSDS) or Safety Data Sheet (SDS) is the source for chemical
hazard information including basic information on the manufacturer or distributor, identifica-
tion of the chemical, the product’s hazardous ingredients, physical data, fire and explosion da-
ta, toxicity information, protection information, and more. The laboratory is responsible for
having a MSDS for every chemical or substance being used. It is also the laboratory’s respon-
sibility to make the MSDS available and accessible to all employees and to provide training in
the safe handling of hazardous chemicals. The MSDS can be obtained from the vendor.

1.2: Product Safety Notice and Certification
3
•All hazardous reagents and chemicals must be disposed in accordance with appropriate Feder-
al, state, and local regulations.
•The SPE-DEX 3100 Oil & Grease Extractor requires the use of an inert pressurized gas source
to pressurize the Solvent Delivery System. The recommended source is a dry grade of nitrogen
gas. If a gas cylinder is used, secure the gas cylinder to avoid tipping.
•The SPE-DEX 3100 Oil & Grease Extractor uses organic solvents that can pose inhalation,
skin, and ingestion hazards with potential chronic health effects. These reagents are also
flammable, which could cause fire and/or explosion hazards. All reagents must be handled us-
ing appropriate personal protection equipment and in a properly operating fume hood to elimi-
nate inhalation hazards. For handling and safety instructions, refer to the Material Safety Data
Sheet (MSDS) for the specific chemical.

1: Introduction and Safety
4
Notes:

5
2 Theory of Operation
2.1 Oil & Grease Extraction
2.1.1 The Goal of Oil & Grease (n-Hexane Extractable Material) Measurement
Oil & Grease is a general hydrocarbon measurement that can indicate the degree of pollution in a
water source. It is described as follows.
•“Oil and grease” is defined as any material recovered as a substance soluble in the solvent. It
includes other material extracted by the solvent from an acidified sample (such as sulfur com-
pounds, certain organic dyes and chlorophyll) and not volatized during the test. (Standard
Methods, 20th Edition)
•The principal types of compounds included in oil and grease analyses are fats, soaps, fatty ac-
ids, hydrocarbons, waxes, and oils. (M.K. Stenstrom, S. Fam, and G. Silverman, Env. Tech.
Letters, 7, 625-636 (1986))
Oil & Grease measurements can be used to indicate pollution for regulatory purposes such as
through the National Pollutant Discharge Elimination System (NPDES) in the US. Based on the
Federal classification category of an industry they might be limited in how much material of this
type can be discharged into a waterway, to help maintain the health of the waterway for recrea-
tional uses.
The measurement may also be used in a wastewater treatment plant to measure their influent
characteristics to ensure the treatment plant operation will not be upset by an unusually high
amount of oil & grease discharged into the sewer system and entering their treatment facility.
Overall, it is a useful general measurement of hydrocarbon pollution.
2.1.2 Methods for Oil and Grease Measurement
There are several methods used around the world specifying n-hexane extraction and
gravimetric measurement of the resulting extracted material.
•US EPA Method 1664: available free of charge from the US EPA website at www.epa.gov.
•Standard Methods 5520B and F(Silica Gel treated Non-polar material): available from Stand-
ard Methods for the Examination of Water and Wastewater. Can be purchased from their
website at https://www.standardmethods.org/
•ISO 11349: ISO standard can be purchased from http://www.iso.org/iso/home/store.htm
These are modern methods developed since the Montreal Protocol required elimination of chloro-
fluorocarbons , such as Freon®, used for extraction in the early days.
Other methods that are generally used when more well-defined information is needed about the
hydrocarbons present in the extract are as follows:
•ISO 9377-2. Extraction and measurement by either gravimetry or GC-FID to determine a hy-
drocarbon oil index
•OSPAR method in Europe. This method extracts with pentane and then uses GC with a flame
ionization detector (FID) to define the range of hydrocarbons that can be measured.

2: Theory of Operation
6
•US EPA 8015 uses methylene chloride for the extraction and GC-FID for analysis. The range
of hydrocarbons includes the broad categories of gasoline-range organics (GRO) and diesel
range organics (DRO).
If information is needed on specific hydrocarbons that might be included in the extract
there are many specific methods that can be used to further characterize the extract and
can be found at many regulatory agency websites around the world, including the US
EPA (www.epa.gov) .
2.1.3 The Role of Solid Phase Extraction (SPE)
Solid phase extraction is a useful tool for extracting oil and grease from a water sample
into hexane solvent so that it can be more readily evaporated and the residual oil and
grease measured gravimetrically.
Solid phase extraction provides advantages over liquid-liquid extraction in:
•Using less solvent, minimizing cost and exposure
•Generating less waste
Solid phase extraction can also be automated, providing other benefits, such as:
•Better precision between analysts
•Excellent recoveries with Pacific Premium disks
•Minimal learning curve for new technicians
2.1.4 Extraction Process Overview
The extraction process is described in the next set of steps.

2.1: Oil & Grease Extraction
7
Step 1. Condition the Disk
The solid phase extraction disk is matched to
the chemistry of the application so that it will
effectively extract the analytes of interest.
The disk needs to be conditioned to prepare it
to accept sample. Generally it is conditioned
with polar solvents when the sample is water.
Step 2. Process the Sample
The sample flows from the original sample
bottle that it was collected into through the
water inlet valve and into the disk holder.
The sample can flow through the disk very
quickly and is then directed to waste.
The analytes of interest (oil & grease/ n-
hexane extractable material) are retained on
the disk.
Step 3. Sample Bottle Rinse
The sample bottle is rinsed with a stream of
solvent that will be used for elution. This en-
sures that any analytes of interest, adhering to
the glass bottle will be carried to the disk and
eluted with the other analytes.
Step 4. Elute the Analytes
Hexane is used to elute the analytes of interest
from the disk into the elution flask or separa-
tory funnel.
The disk is rinsed to ensure a good transfer
and recovery of the analytes.
The eluent can then be dried and transferred
to a pan to evaporate the hexane, leaving be-
hind the oil and grease residue, which is then
measured gravimetrically.

2: Theory of Operation
8
Notes:

9
Part I:
Getting Started

10