InfraCal 2 TRANS-SP User's Guide

Measuring Oil and Grease from Water and Soil

Doc p/n 100-00323

Rev. B | January 2019

Spectro Scientific - An ISO 9001:2015 Company

One Executive Drive, Suite 101, Chelmsford, MA 01824-2563. Tel. (+1) 978 431 1120
www.spectrosci.com
 Preface
This section provides information about Spectro Scientific and the InfraCal 2 fluid analyzer.

Copyright Notice
© 2019 Spectro Scientific. All rights reserved.
The information and descriptions in this document are the sole property of Spectro Scientific and
may not be copied, reproduced, disseminated, or distributed without explicit written permission from
Spectro Scientific.
The statements, configurations, technical data, and recommendations in this document are believed
to be accurate and reliable at the time of this publication, but Spectro Scientific assumes no
responsibility or liability for any errors or inaccuracies that may appear in this document.
Spectro Scientific is not responsible for any infringement of patents or other rights of third parties
that may result from the use of this document. The content of this document is furnished for
informational purposes only, is subject to change without notice, and does not represent a
commitment or guaranty by Spectro Scientific.
Spectro Scientific makes no warranty, express or implied, with respect to the content of this
document. Spectro Scientific shall not be liable for any loss or damage, including consequential or
special damages, resulting from any use of this information, even if loss or damage is caused by
Spectro Scientific as a result of negligence or any other fault.

Warranty
There are no user-serviceable parts inside. Opening the case will void the
warranty.
Use of any other power supply than the one provided will void the warranty.
Spectro Scientific warrants to the original purchaser that all Spectro Scientific portable instruments
will be free from defects in material or workmanship for a period of one year from date of invoice.
Spectro Scientific's sole obligation and your exclusive remedy under this Limited Warranty and, to
the extent permitted by law, any warranty or condition implied by law, shall be the repair or
replacement of parts, without charge, that are defective in material or workmanship and that have
not been misused, carelessly handled, abnormal conditions or operation, accidents or acts of God,
or misrepaired by persons other than Spectro Scientific or Authorized Service Provider.
To make a claim under this Limited Warranty, you must return the complete portable instrument,
transportation prepaid, to Spectro Scientific Factory Service Center or Authorized Service Location.
The determination of whether any product has been subject to misuse or abuse will be made solely
by Spectro Scientific. If a hardware defect arises and a valid claim is received within the limited
warranty period, at its option and to the extent permitted by law, Spectro Scientific will either:

(1) repair the hardware defect at no charge, using new parts or refurbished parts that are equivalent
to new in performance and reliability or
(2) exchange the product with a product that is new or refurbished that is equivalent to new in
performance and reliability and is at least functionally equivalent to the original product, or
(3) refund the purchase price of the product.

i
Spectro Scientific may request that you replace defective parts with user-installable new or
refurbished parts that Spectro Scientific provides in fulfillment of its warranty obligation. A
replacement product or part, including a user-installable part that has been installed in
accordance with instructions provided by Spectro Scientific, assumes the remaining warranty of
the original product.
After an issue with the unit has been verified, the offending module where the issue originates
should be returned to the factory for repair by authorized Spectro personnel.

Spectro Scientific Phone Numbers

Main Number (U.S.) (+1) 978-486-0123
Technical Support: (U.S.) (+1) 978-431-1130
Main Number (China) - 8610-6785-7242

Trademarks
FluidScan®, MicroLab®,InfraCal®, LubeTrak® and Spectro Scientific® are all registered
trademarks of Spectro Scientific.
SpectroTM, SpectroViscTM, SpectroTrakTM, SpectroLNFTM, SpectroFTIRTM and SpectroFDMTM
are all unregistered trademarks of Spectro Scientific.
All other trademarks are the property of their holders.

Patents
Domestic
9,274,041; 9,234,829; 9,176,041; 8,867,034; 8,661,878; 8,384,895; 8,079,250; 7,518,720;
7,495,761; 7,385,694; 7,307,717; 7,237,431; 7,184,141; 7,019,834; 6,873,411; 6,707,043;
6,455,850; 6,452,179; 6,104,483; 2,640,059; 2,340,097.

Foreign
163,024; 141,344; P5707513; EP1105710B1; AU2003257512B2; AU199953978B2.

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 Document Conventions
There are three types of special instructions that appear in this manual. They are there to protect the
user and the device and also to emphasize key points or instructions.

An operating procedure or practice that may cause damage to the device, injury to
the user, or a gross impact on testing or analyzing results.

An operating procedure or practice that may have an impact on testing or

analyzing results.

An item worthy of special note that may amplify information already given.

Safety Information
The safe and proper operation of the InfraCal 2 is our highest priority. The device must be used by
trained operators, according to the instructions presented in this manual.
Improper use could cause physical harm or damage to the device. Pay attention to all warning labels
and messages.

Personal Precautions
We recommend that you wear appropriate safety equipment such as gloves and safety goggles.

Environmental Precautions
Do not allow fluids to enter groundwater or sewers.
In the event of a spill,
1. Apply an absorbent material to the spill
2. Place the material in an appropriate chemical waste container
3. Follow local, state, and federal regulations for disposal

Document Revision History

Rev Date Description
A March 2017 First release under Spectro banner
B January 2019 Forklift update of all sections,plus the addition of all appendices.

iii
End User License Agreement (EULA)
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"Software” means computer programs provided to Licensee by SPECTRO SCIENTIFIC directly
or indirectly, and any related materials, including, but not limited to, Documentation related
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which the Software is provided by Spectro.

2. Scope of Authorized Use

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the Licensee's own use only on the Spectro Single unit ("Unit") on which Software is first
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ate Software due to an equipment malfunction, the Software may be used temporarily on
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Licensee shall pay invoiced license fees, including tax on the license fee, for use of the Software,
within thirty (30) days after shipment.

iv
5. Limited Warranty: Warranty Disclaimer
SPECTRO SCIENTIFIC warrants that all Software will substantially conform, for a period of thirty
(30) days from shipment, to SPECTRO SCIENTIFIC's specifications prevailing at shipment.
SPECTRO SCIENTIFIC does not warrant Software will be error free or that all errors will be
remedied.
SPECTRO SCIENTIFIC's entire liability and Licensee's exclusive remedy under this warranty shall
be for SPECTRO SCIENTIFIC to make reasonable efforts to remedy, in a manner deemed suitable
to SPECTRO SCIENTIFIC, any non-conformance reported in writing within the warranty period.
NEITHER SPECTRO SCIENTIFIC NOR ITS THIRD PARTY VENDOR (IF ANY) MAKE OR
GIVE, AND SPECTRO SCIENTIFIC HEREBY DISCLAIMS, ANY OTHER REPRESENTATION
OR WARRANTY REGARDING THE SOFTWARE, INCLUDING EXPRESS OR IMPLIED
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OPERATES ON ARE BEING PROVIDED HEREUNDER FOR OIL ANALYZING ACTIVITIES
ONLY AND SPECTRO SCIENTIFIC HAS NO LIABILITY OR RESPONSIBILITY TO PROVIDE
INFORMATION OR DATA RELATED TO THE OPERATION OR CONDITION OF EQUIPMENT
OR MACHINERY BEING OPERATED.

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SPECTRO SCIENTIFIC disclaims all liability for copyright, patent or other infringement, including
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8.1 Licenses shall become effective upon Software shipment and terminate at such time as
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immediately return or destroy at SPECTRO SCIENTIFIC’s direction all copies of such Software
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v
9. Miscellaneous
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excluding choice of law provisions and Licensee agrees that the exclusive proper venue for all
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ation, without first complying with all applicable export laws and regulations.
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any conflicting contractual terms or conditions.
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SPECTRO SCIENTIFIC.
The following additional statement applies only to acquisitions governed by DFARS Subpart
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subject to restrictions as set forth in subparagraph (c)(1)(ii) of the Rights in Technical Data and
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vi
 Table of Contents
Copyright Notice i
Warranty i
Spectro Scientific Phone Numbers ii
Trademarks ii
Patents ii
Domestic ii
Foreign ii
Document Conventions iii
Safety Information iii
Personal Precautions iii
Environmental Precautions iii
Document Revision History iii
1. Definitions iv
2. Scope of Authorized Use iv
3. Title and Ownership: Confidentiality iv
4. Payment, Shipment, and Risk of Loss iv
5. Limited Warranty: Warranty Disclaimer v
6. Limitation of Remedies v
7. Infringement Indemnity v
8. Termination v
9. Miscellaneous vi
1 Introduction 1
TRANS-SP Theory of Operation 1
2 Quick Reference Guide 2
Clean the Cuvette. 2
Zero the Instrument 2
Test the Sample 2
3 Getting Started 3
Unpacking the Shipping Carton 3
Installation Location 3
Power Requirements 3
Activating the Internal Battery 3
External Connectors 4
Powering On/Off 4
Warm-Up Time 4
Touch Screen Interface Description 5
Main Menu Overview 5
Navigating Tables 7
Using Drop-Down Menus 7
Entering Text and Numbers 8

vii
 Setting the User Interface Language 8
Setting the Date, Time and Daylight Savings Time 8
Setting Battery Stretch and Display Brightness 9
4 Administrative Functions 10
Adding a Security PIN to the Default Admin 10
Changing Users 11
Adding a New User 12
Editing Existing Users 13
Deleting Users 13
Adding Data Labels 13
Selecting a Calibration 14
Editing a Calibration 14
Deleting a Calibration 15
Reviewing Saved Measurements 15
Exporting Saved Measurements 16
Deleting Saved Measurements 17
Updating the Software 18
5 Creating a Calibration 19
Creating a New Calibration 19
Measuring Calibration Standards 22
Graphing the Calibration Points 24
6 Testing Samples with the TRANS-SP 25
Solvents 25
Sample Extraction Materials 26
Oil in Water Extraction Materials 26
Oil in Soil Extraction Materials 27
Measuring Oil in Water Samples 27
Extraction Method 27
Separating Solvents Heavier than Water 28
Measuring Oil in Soil Samples 28
Extraction Method 28
Cleaning the Cuvette 29
Zeroing the Analyzer 29
Analyzing a Sample 30
7 Accessing Diagnostic Screens 33
Device Information Screen 33
Hardware Information Screen 33
Hardware Diagnostics Screen 34
Power Level Detector Signals Screen 34
A Correlation to Alternate Method 36
B Calibration Standard Preparation 37
Required Materials 37

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 Preparing a Stock Solution 37
Preparing Calibration Standards 38
C Emulsion Breaking Techniques 39
D Diluting a Sample 41
E InfraCal 2 General Theory of Operation 42
Infrared Spectra for Analysis of Chemical Functions 42
Sampling Cell Description 42
F Specifications 43

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 1 Introduction
TRANS-SP Theory of Operation

See also InfraCal 2 General Theory of Operation on page 42 for further

information.

The InfraCal 2 TRANS-SP analyzer is designed to measure solvent extractable material (oil and
grease) by infrared determination in water or soil using tetrachloroethlyene, S-316, AK-225 or
Freon-113 for the extraction procedure. A detector with a fixed 3.4 µm (2940 cm-1) filter is used
to measure oil and grease concentrations.
The TRANS-SP complies with ASTM D7066 as well as EPA 413.1 and 4218.1.
The TRANS-SP makes use of the fact that oil and grease can be extracted from water or soil
through the use of an appropriate solvent and extraction procedure. The extracted hydrocarbons
absorb infrared energy at a specific wavelength and the amount of energy absorbed is pro-
portional to the concentration of hydrocarbons in the solvent. The analyzer can be calibrated to
read out directly in the desired units such as %, ppm, mg/L or mg/kg.
The touchscreen display includes the capability for multiple calibrations, a wizard guide for cal-
ibration, multilevel user database, multiple languages with user preference selection, high/low
alarm and control limits, and measurements stored in a history table for recall or export to a flash
or serial port.

1
 2 Quick Reference Guide
Allow at least 30 minutes for the instrument to warm up. Allow more time if the
instrument is not in a climate-controlled room.
If you have any custom calibrations, tap Analysis and select a calibration from the
table and tap Done. Otherwise the default configuration will apply.

Clean the Cuvette.

1. Fill the cuvette with clean solvent by either pouring directly from the bottle or using a clean,
glass pipette. If measuring samples below 10 ppm, it is recommended to use a clean, glass
syringe with a particle filter attached when filling the cuvette with clean solvent in order to
remove any dust.
2. Empty the contents of the cuvette.
3. Repeat steps 1 and 2.

Zero the Instrument

1. Fill the cuvette with clean solvent by either pouring directly from the bottle or using a clean,
glass pipette. If measuring samples below 10 ppm, it is recommended to use a clean, glass
syringe with a particle filter attached when filling the cuvette with clean solvent in order to
remove any dust.
2. Cap the cuvette immediately.
3. Clean the clear sides of the cuvette by applying clean solvent and gently wiping the cuvette
dry with a Kimwipe.
4. Place the cuvette into the instrument; ensure the frosted sides face forwards.
5. Tap Zero. Do NOT skip the timer.
6. Tap Set Zero and then tap Done.

Test the Sample

1. Extract the sample.
2. Using a clean syringe or a clean, glass pipette, fill the cuvette with the extract approximately
halfway up, then cap the cuvette.
3. Shake the cuvette for 5 seconds and then empty out the contents.
4. Using a clean syringe or a clean, glass pipette, fill the cuvette with the extract at least 3/4 of
the way up, then cap the cuvette.
5. Clean the clear sides of the cuvette with clean solvent and gently wipe dry with a Kimwipe.
6. Place the cuvette into the instrument; ensure the frosted sides face forwards.
7. Tap Run. Do NOT skip the timer.
8. The device will display the concentration on the screen once the measurement is done.

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 3 Getting Started
Unpacking the Shipping Carton on page 3
Installation Location on page 3
External Connectors on page 4
Powering On/Off on page 4
Touch Screen Interface Description on page 5
Main Menu Overview on page 5
Navigating Tables on page 7
Using Drop-Down Menus on page 7
Entering Text and Numbers on page 8
Setting the User Interface Language on page 8
Setting the Date, Time and Daylight Savings Time on page 8
Setting Battery Stretch and Display Brightness on page 9

Unpacking the Shipping Carton

Unpack the shipping carton and compare the contents to the packing list. If they do not match,
contact Spectro Scientific immediately.

Installation Location
The InfraCal 2 Analyzer is designed for on-site measurements and is relatively insensitive to
vibration and ambient temperature changes. For more sensitive readings below 1 ppm, it is best
to avoid dramatic temperature changes such as direct sunlight or a location in the direct air flow of
a heating or air conditioning vent.

Power Requirements

Use of any other power supply than the one provided will void the warranty.

A standard 18 volt power supply is provided as standard and an optional internal battery pack is
available at the time of purchase. The analyzer may be operated from any grounded utility outlet
of 100 - 250 VAC, 50-60 Hz, 2.1 A minimum. When operating, the device uses 0.5 A (up to 2.1 A
with the internal battery charging).

Activating the Internal Battery

The battery will not begin to charge until after the first time you power the device up using the
charger/adapter. After this, you can power the device down and the battery will continue to
charge as long as the power supply is plugged in.

3
 Flip the device over and set the battery slide switch to ON; otherwise, the battery
will not charge:

Allow a new battery to charge for 3 hours before using the device on the internal battery alone.

External Connectors
The following are located on the right side and back of the device:

Powering On/Off
1. Connect the DC side of the power supply to the 18 VDC connector on the back of the
device.
2. Connect the AC side of the power supply to the utility power connector or other appropriate
AC power source.
3. Press the ON/OFF button to turn the instrument on. Press again to turn the instrument off. If
the instrument fails to turn off, press and hold the ON/OFF button until the instrument
powers down (about 5 seconds). No settings will be lost.

Warm-Up Time
For normal operation, it is recommended that the instrument be allowed to warm up for 1 hour prior
to use. The InfraCal 2 Analyzer draws very little power and, if used daily, it can be left on at all times
(unless you are using the internal battery pack only).

4
Touch Screen Interface Description
The user interface is a resistance type LCD touch screen. Commands are best activated with a
resistance screen stylus, pencil eraser or fingertip.

Damage to the touchscreen by the use of sharp objects is not covered by the
warranty.

While resistant to many chemicals, it is best to avoid chemical contact with the screen surface.
The surface can be cleaned with a soft cloth and, if necessary, with some plastic surface cleaner
applied to the cloth.

Main Menu Overview

The Main Menu will open similar to this example:

1 - Instrument Status - Displays the following status messages:

• History table full. Readings will not be recorded
• Instrument has not been zeroed.
• Instrument is ready.

Test samples only when the Instrument is Ready message is displayed.

2 - Units of Measure - TRANS-SP output is in ppm.

5
3. Test Result - Displays the test result to the number of decimal places specified in the calibration.
4. Target Concentration - Optionally configured as part of the alarm, it must be less than the
Upper Control Limit and greater than the Lower Control Limit.
5. Calibration Name - By default, the device will re-open to the calibration in use when it was
powered down last.
6. Power Indicator - Indicates whether the device is running on utility AC power using the
adapter/charger, or on internal battery power.
7. User Name: Indicates who is logged in. Three users are configured by default: You can perform
all tasks described in this guide with just these default users without ever adding any new users. If
you want to add more users, see Adding a New User on page 12 for information.

• Admin User: Full unrestricted access except to the Factory User configuration.
• General User: Can run samples, change the screen language and change display
brightness/battery stretch function. Can view - but not edit - the sample history, any custom
configuration analysis details, and any other users.
• Factory User: For Spectro Support Services use only.
8. Alarm Scale: If alarms are created as part of a calibration, the alarm limits will be displayed in
colored bars. The scale minimum and maximum values are also defined in the calibration.
9. Action Buttons: Menus and sub-menus are accessed by tapping the navigation buttons that
run across the bottom of each menu.
Blue buttons are active and they suggest the next action, such as Zero the Instrument:

Light gray buttons are also active and they indicate there is an alternate option to a blue button. In
this example, although the software is suggesting you zero the instrument, you could open the
Setup menu and add a new user:

Dark gray buttons are always inactive in the current menu, but they can be activated as part of
another process, such as exporting test results to a USB memory stick.
For example, the Flash button is always inactive until a USB memory stick is inserted:

When a USB memory stick is detected, the button will change to light gray to indicate that sending
data to the USB memory is now an available option:

6
Navigating Tables
Whenever you see a table like this example, you can select any entry by tapping it to highlight the
field in blue:

You can see a maximum of 4 - 5 line items in any table - if you have more, you
need to swipe up or down with your finger as you would with a cell phone.
There are usually hidden columns, so you can tap the blue arrow buttons to
move left or right.
You can tap the header at the top of any column to sort it from A to Z or from Z
to A, or from High to Low or Low to High.

Using Drop-Down Menus

A drop-down menu is indicated by a blue down-arrow next to a field. Tap the down-arrow and
options will be revealed; for example, a list of user names. Tap the user you want to select - for
this example, select Admin user:

7
Entering Text and Numbers
You can enter alpha-numeric text in any blank box by tapping in it to open a software keyboard. Tap
in your entries and tap Enter to close the keyboard.
Certain fields - creating or entering a PIN for example - will open a calculator-style numbers only
keypad:

ESC: Returns you to the previous screen.

C: Clears the numbers area
<: Backspace
=: Enter selection

Setting the User Interface Language

This only changes the language temporarily. If the instrument is restarted, then the language will go
back to the user default.

In order to permanently set the language for a particular user, set the language
when you create the new user. See Adding a New User on page 12 for details.

1. From the Main Menu, tap the Setup button.

2. Tap the down arrow for the Language field and scroll through the languages and select the
one you want. Current options are Spanish, French, Portuguese, Arabic or Chinese.
3. Tap the Done button. The entire user interface is now displayed in the selected language.

Setting the Date, Time and Daylight Savings Time

1. From the Main Menu, tap the Setup button.
2. Tap the More button.
3. Tap the Clock button.

8
 4. Tap the Up and Down buttons to set the correct time:

Setting Battery Stretch and Display Brightness

To stretch the battery life, you can dim the display, as follows:
1. From the Main Menu, tap the Setup button.
2. In the Display Brightness field, tap the arrow and tap Power Save.
3. Tap Done. The screen will dim immediately.

9
 4 Administrative Functions
This section describes more advanced functions for operating your instrument.
Adding a Security PIN to the Default Admin on page 10
Changing Users on page 11
Adding a New User on page 12
Editing Existing Users on page 13
Deleting Users on page 13
Adding Data Labels on page 13
Selecting a Calibration on page 14
Editing a Calibration on page 14
Deleting a Calibration on page 15
Reviewing Saved Measurements on page 15
Exporting Saved Measurements on page 16
Deleting Saved Measurements on page 17
Updating the Software on page 18

Adding a Security PIN to the Default Admin

You must be logged in as an Admin user to perform this task.

By default, the last user logged in before the device was powered down will be
logged in again on restart. If the last user had Admin privileges without requiring
a PIN, everyone now has unrestricted access.
We strongly recommend a PIN for all Admin-level users. Adding a PIN to the
default Admin will enforce this for Admin-level users you create and General
users who become Admins.

1. From the Main Menu, tap the Setup button to enter the Setup Menu.
2. From the Setup Menu drop-down list, tap Admin user to select:

3. Tap the Security button.

10
 4. From the Security Menu, tap the Admin user entry to highlight it:

5. Underneath the users is the PIN Required option. Tap the blue Admin radio button to select
it:

6. Tap the Edit button, then tap in the PIN field:

7. A calculator-style keypad opens. Create a PIN with a minimum of 4 numbers and tap = to
enter the selection.
8. Tap Done three times to back out to the Main Menu.

You are still logged in as the Admin. To fully set log-in protection you need to tap
the Setup button and select the General user to log out as Admin. Then tap Done.

Every Admin-level user you create from this point, and any General users who become Admin-level
users, will now be required to have a PIN.

Changing Users
You can see who is currently logged in by looking at the top right corner under the Date and Time
field. Unless you add new users as described later in this section, you can only change between the
default Admin User and the default General User.
1. From the Main Menu tap the Setup button.
2. Tap the down arrow next to the User Name field and select the user to change to:

11
 3. Tap Done to change user and change the name in the upper right corner.

Adding a New User

You must be logged in as an Admin-level user.
1. From the Main Menu, tap the Setup button.
2. Tap the Security button to open the Security Menu:
3. Tap the Security button to open the Security Menu:

4. If a PIN is required for all Admin users, press the Admin radio button in the Pin Required
section; otherwise press None. Do not select the All option:

5. Tap the New button.

6. Tap the User Name field to open a software keyboard and enter a name. For this
example, enter John J:

7. Click the down-arrow next to the Type field and select either Admin or General as your
user type. If you selected General, go to Step 9.
For this example, John J is a new Admin and a PIN is required for all Admins. Tap in the
PIN field to open a keypad.
8. Create a PIN (minimum of 4 digits) and press = to enter.

12
 9. Tap the down arrow in the Language field to select a permanent default language for this
user. Current options are English, Spanish, French, Portuguese, Arabic or Chinese.
10. Tap the down arrow in the Timeout field. This sets for how long the user has access before
having to re-authenticate with the PIN. We recommend every 8 Hours for Admin users and
Never for General users.
11. Tap the Done button to create the user and return to the Security screen.

Editing Existing Users

You must be logged in as an Admin-level user. Admin-level users can edit all other users except the
Factory user.
If you have more than 5 users in the table, you can swipe up or down similar to a cellphone to see
them all. You can also tap the left and right arrows to see all the columns.
Tap on any column header to sort A-Z or Z-A, Newest-Oldest or Oldest-Newest.
1. From the Main Menu, tap the Setup button.
2. From the Setup Menu, tap the Security button.
3. Tap the user you want to edit.
4. Tap the Edit button, make your changes, and tap the Done button.

Deleting Users
You must be logged in as an Admin-level user.
Admins can delete General users and other Admins. There will always be at least one Admin user
so you can't accidentally lock yourself out.
If you have more than 5 users, you will have to swipe up or down to see them all. Tap on any column
header to sort A-Z or Z-A, Newest-Oldest or Oldest-Newest.
1. From the Main Menu, tap the Setup button.
2. From the Setup Menu, tap the Security button.
3. Tap the user you want to delete to highlight the row.
4. Tap the Delete button, then tap Done.

Adding Data Labels

You have the option to add up to 2 labels to describe a sample. For example, you might add a
Sample ID for Label 1 and a description of the equipment the sample came from for Label 2.

Data labels will be attached to all measurements until they are either cleared or
changed.

1. From the Main Menu, tap the Setup button.

2. Tap the More button.

13
 3. Tap the Data button to open the Label screen:

4. Tap inside the white box for Label 1 to open a keyboard to add a descriptive label:

5. Optional: Tap the Label 2 field to add a second label.

6. Tap the Done button.

Selecting a Calibration
Your instrument may ship with a factory calibration. You can also create one or more custom cal-
ibrations (see Creating a New Calibration on page 19 for details).
You can then switch between them by following these steps:
1. From the Main Menu, tap the Analysis button to open a screen similar to this example:

Each calibration has one of three possible icons displayed:

2. Tap any good calibration and tap Done.

Editing a Calibration
You must be logged in as an Admin-level user.
1. Tap the Analysis button.

14
 2. Tap the calibration to be edited.
• If the middle button says Edit, any Admin user can edit all settings for any Custom
calibration
• If the middle button says Details, an Admin user can only edit the following fields in a
Factory calibration:
Precision, Units, Alarm Limits, Scale Factor.
General users have no editing rights, but can view the calibration settings by pressing the
Details button.

Deleting a Calibration
You must be logged in as an Admin-level user.
1. From the Main Menu, tap the Analysis button to open an Analysis menu similar to this
example:

2. Tap the calibration you want to delete.

If you have access to the calibration, the Delete button will be active (light gray) as
shown above. Tap the Delete button, and then tap the Delete button that appears in the
pop-up in order to delete the calibration.
If you do not have access to the calibration, the Delete button will be inactive (dark
gray).

Reviewing Saved Measurements

1. From the Main Menu, tap the History button to open a History menu similar to this example:

15
 2. There are 4 types if measurements that can be displayed:
• Gear symbol with green check-mark: This symbol indicates a Zero measurement that
was Set.
• Gear symbol with red X: This symbol indicates a Zero measurement that was Not Set.
• Magnifier with grey X: This symbol indicates the result is from a single measurement.
• Magnifier with grey +: This symbol indicates the result is the average of all
measurements taken during a continuous measurement. You may select this result and
press the Details button in order to see each recorded measurement in the series.
If you have more than 5 results, swipe up or down to scroll through them.
Press and swipe the blue right arrow to scroll to the right to see more data columns.
Tap any column header to sort results from A to Z or Z to A, Oldest to Newest or Newest to
Oldest.

Exporting Saved Measurements

1. From the Main Menu, tap the History button.
2. The History screen opens similar to this example:

3. Follow these steps to export the results to either a computer or USB Flash Drive:
• To export results to a computer, connect the device to the computer using a USB-A to
mini-B cable. Then contact Spectro Support Services for assistance with setting up a
terminal emulation program and completing the process.
• To export results to a USB Flash Drive, plug the drive into the USB slot on the right side
of the analyzer. The Flash button will turn from inactive (dark gray) to active (light gray):

16
Tap the measurement you want to export to select it. You may also select all measurements by
tapping anywhere in the left column:

Selecting multiple results is not supported. Select one result or all results.

4. Beneath the list of results, tap the button to select the output format. You can export your
data as Formatted, which is a formatted text file, or as a .csv file.
You can export data as both, but not simultaneously.
5. Tap Flash to send the data to the Flash drive.

Deleting Saved Measurements

Up to 2,000 measurements are saved automatically. When the History Table is full, the following
message will display in the Main Menu: History table full. Readings will not be recorded.
You will need to clear some space to continue.
You must be logged in as an Admin-level user.
1. From the Main Menu, tap the History button. The History screen opens similar to this
example:

17
 2. Tap the entry you want to delete to select it. Otherwise, you can select all saved
measurements by tapping anywhere in the left column:

Selecting multiple results is not supported. Select one result or all results.

3. Tap the Delete button, then confirm you want to delete the measurement(s).

Updating the Software

You must be logged in as an Admin-level user.

This procedure may delete the History Table. We recommend that you
create a backup copy on a USB Flash Drive before continuing.
In order to update software, the power supply/charger must be connected to
utility or generator power.
Do not disconnect the power supply/charger while the update is in progress.
Do not shut down the analyzer while the update is in progress.

1. Copy the new software to a USB Flash Drive and plug it into the USB port on the side of
the device.
2. From the Main Menu, tap the Setup button.
3. Tap the More button.
4. When the device detects the new software, tap the Software button to start a series of
compatibility checks.
5. Once the checks are complete, tap Update and then confirm; this will install the new
software.

18
 5 Creating a Calibration
This chapter describes the following:
Creating a New Calibration on page 19
Measuring Calibration Standards on page 22
Graphing the Calibration Points on page 24

Creating a New Calibration

You must be logged in as an Admin-level user.
1. From the Main Menu, tap the Analysis button to open the Analysis Menu.
2. From the Analysis Menu, tap New to open a menu similar to this example:

Analysis Name: Tap in the field to open a software keyboard and create a unique name for this
configuration.
Created by: Not accessible. This is a default field.
Calculation Method: Tap the down arrow and select Table.
Precision: Tap the down arrow and select the number of digits to display to the right of the decimal
point, as follows:
• If you intend to set the Maximum Range field (see below) to 10 ppm or less, select XXXX. X
• If you intend to set the Maximum Range field above 10 ppm, select XXXXX.
Units: Tap the down arrow and select the units of measure, as follows:
For oil in water measurements, use either mg/l or ppm.
For oil in soil measurements, use mg/kg.
3. Tap Next to open a menu similar to this example:

Run Countdown Timer - Sample measurement start is delayed by the selected time. Tap the
down arrow to select a value.
• If you intend to set the Maximum Range field to 10 ppm or less, select 4 minutes
• If you intend to set the Maximum Range field above 10 ppm, select 2 minutes.

19
Zero Countdown Timer - Zero measurement start is delayed by the selected time. Tap the
down arrow to select a value.
• If you intend to set the Maximum Range field to 10 ppm or less, select 4 minutes
• If you intend to set the Maximum Range field above 10 ppm, select 2 minutes.
Measurement Avg - Select the average sample measurement time from 10 - 30 seconds. 30
seconds is recommended.
Zero Expiration - The default setting is that the zero never expires. Optionally, tap the down
arrow and set a timer to force the zero to expire at the specified time.
Calibration Expiration - The default is that the calibration never expires. Optionally, tap the
down arrow and set a timer to force the calibration to expire at the specified time.
Skip Check-box - Tap this box to activate a Skip button in the appropriate screens when
running a sample or zeroing the device.
Today Check-box - Tap this check-box to begin calculating the expiration time from today’s
date.
4. Tap Next to open the following menu:

Analytical - Not accessible - default only.

Reference 1 - Not accessible - default only.
Reference 2 - Not accessible - default only.
Maximum Range - Enter the maximum calibration range. The maximum range should not
exceed the Concentration value of the highest standard.
Minimum Range - Enter the minimum calibration range. Measurement results below this limit
will display in red.
5. Tap Next to open the Alarms menu. Alarm limits can be set as described below, or tap
Done to continue without setting any alarms:

20
Beep Check-Box - Tap the check-box to sound an audible alarm when the alarm limit is reached.
Upper Alarm Limit - Tap the check-box to activate. Tap the Value field to set the limit which must
be less than the Maximum range. This will cause a result in this range to be displayed in red.
Upper Control Limit - Tap the check-box to activate. Tap the Value field to set the limit which must
be less than the Upper Alarm Limit. This will cause a result in this range to be displayed in yellow.
Target - Tap the check-box to activate. Tap the Value field to set the limit which must be less than
the Upper Control Limit and greater than the Lower Control Limit. This will cause a result in this
range to be displayed in green.
Lower Control Limit - Tap the check-box to activate. Tap the Value field to set the limit which must
be greater than the Lower Alarm Limit. This will cause a result in this range to be displayed in yellow.
Lower Alarm Limit - Tap the check-box to activate. Tap the Value field to set the limit which must
be greater than the Minimum Range. This will cause a result in this range to be displayed in red.
6. Tap Next to open the Calibration Points table similar to this example. Calibration standards
data usually found on the bottles can be entered directly into this table:

For making manual entries directly in the table, you must have the Absorbance
and Concentration values for each calibration standard to continue with this sec-
tion.
If you do not have these available, enter 0 in all fields for Point 1 and tap the Curve
button. Then refer to Measuring Calibration Standards on page 22 to continue
adding point data starting with Point 2.

Absorbance: The absorbance for each calibration standard is listed in this column. To add or edit a
value, tap the appropriate field in the Absorbance column and enter/edit the desired value.
Concentration: The concentration for each calibration standard is listed in this column. To add or
edit a value, tap the appropriate field in the Concentration column and enter/edit the desired value
Scale x 1.0000: Multiplication factor for listed concentrations. Each row in the Scale Factor column
will show the corresponding concentration value multiplied by this factor. The default value for this
column should be 1. To change this value, select the column and enter a new multiplication factor.
We recommend you contact Spectro Support Services for assistance with this.

21
A completed table after entering the data for 3 standards might look similar to this example:

The calibration is complete. Tap Done to return to the Main Menu.

Optional: Tap the Graph icon to display the table entries as a graph. See Graphing
the Calibration Points on page 24 for details.

Measuring Calibration Standards

If you do not have the Absorbance and Concentration values for each of the calibration
standards, you can generate values in this screen and add them to the Calibration Points table
directly by pressing the Add button:

1. Clean the cuvette. See Creating a Calibration on page 19 for details.

2. Zero the instrument. See Zero the Instrument on page 2 for details.

The device must be zeroed between each standard. For calibrations

configured with a Maximum Range below 10 ppm, you must use the same
cuvette for the standard as you use for the zero.

3. Fill the cuvette with the first standard and cap the cuvette immediately.
4. Clean off the clear sides of the cuvette with clean solvent and wipe dry with Kimwipes.
5. Place the cuvette into the instrument with the frosted sides facing forward.
6. Tap the Run button. A result will appear in both the result box and along the left side of
the screen similar to this example:

Notice that the output in the gray result box only supports 4 decimal places. In
all other places, the output is displayed to 5 decimal places.

22
 7. Remove the cuvette for 1 minute.
8. Place the cuvette back into the instrument and run a second sample of the same standard.
The screen now looks similar to this example. Note the average at the bottom of the screen -
the blue checkbox next to a measurement means it is included in this average:

9. Remove the cuvette for 1 minute.

10. Place the cuvette back into the instrument and run a third sample of the same standard.
The screen now looks similar to this example.

If one of your measurements is obviously out of range high or low, you can
remove it from the average by un-checking the blue box. Then run another
sample to replace it.

11. Tap the Value button and enter the Concentration value of the first standard. For this
example, enter 10.
12. Tap the Add button to add the average - 0.11060 - to the Calibration Points table for Point 2.
13. Repeat this process for the remaining standards for points 3 and 4. For this example,
assume they have a Concentration value of 25 (Point 3) and 50 (Point 4).

23
The calibration is complete.
Optional: Tap the Back button to view the Calibration Table. A Calibration Table after measuring
the 3 standards could look similar to this example:

Optional: Tap the Graph icon to display the table entries as a graph. See Graphing
the Calibration Points below for details.
Tap Done to return to the Main Menu.

Graphing the Calibration Points

A visual representation of the calibration points curve is available by pressing the blue Graph icon
in the Calibration Points table. A curve might look similar to this example:

24
 6 Testing Samples with the TRANS-SP
This section describes the following
Solvents on page 25
Sample Extraction Materials on page 26
Oil in Water Extraction Materials on page 26
Oil in Soil Extraction Materials on page 27
Measuring Oil in Water Samples on page 27
Separating Solvents Heavier than Water on page 28
Measuring Oil in Soil Samples on page 28
Cleaning the Cuvette on page 29
Zeroing the Analyzer on page 29
Analyzing a Sample on page 30

Solvents

We recommend the following solvents. Contact Spectro Support Services if you

wish to use a different solvent.

S-316: A proprietary, non-hydrocarbon solvent said by its manufacture to be environmentally safe. It

is the solvent used in ASTM D7066. Since it is heavier than water, the solvent after extraction will be
on the bottom requiring a separatory funnel or syringe with an inverted sample bottle with a septa
cap. Because of its infrared transparency, it can be used with a 10mm quartz cuvette. Because no
evaporation step is required light end volatiles will be retained for measurement
Tetrachloroethylene: A common replacement for Freon-113. Since it is heavier than water, the
solvent after extraction will be on the bottom requiring a separatory funnel or syringe with an inver-
ted sample bottle with a septa cap. Because of its infrared transparency, it can be used with a 10
mm quartz cuvette. Because no evaporation step is required, light end volatiles will be retained for
measurement.
Many grades are stabilized with hydrocarbons making them unsuitable for TOG and TPH analysis.
The only hydrocarbon-free grade we have found suitable is J.T. Baker’s Tetrachloroethylene
ULTRA RESI-ANALYZED (Perchloroethylene) product # 9360.
Freon-113: Specified for EPA Methods 413.2 and 418.1. Freon-113 may not be available in many
parts of the world due to being banned in the Montreal Protocol. Since it is heavier than water, the
solvent after extraction will be on the bottom requiring a separatory funnel or syringe with an inver-
ted sample bottle with a septa cap.
Because of its infrared transparency, it can be used with a 10mm quartz cuvette. Because no evap-
oration step is required light end volatiles will be retained for measurement. Freon is ideal for applic-
ations requiring the measurement of light ends, as well as, the heavier components in water and soil
samples.

25
Sample Extraction Materials
The following are required for both Oil in Water and Oil in Soil measurements.
1. 25 ml graduated cylinder.
2. Sodium sulphate (Na2SO4) ACS, granular anhydrous (TOG/FOG analysis only).
3. 125 mL Teflon wash bottle.
4. Glass Funnel.
5. Whatman 40 Filter paper, 11 cm or equivalent.
6. Silica gel, anhydrous, 75 - 150 μm (TPH analysis only).
7. 10 mm quartz cuvette.
8. Solvent.

Oil in Water Extraction Materials

One of the following:

• 100 mL stoppered graduated cylinder (for solvents lighter than water).
• 125 mL stoppered separatory funnel or sample bottles with septa caps (for solvents
heavier than water).
177-ml prescription bottles (for solvents both lighter than or heavier than water).
Disposable polyethylene pipette or equivalent
5 mL syringe (for use with prescription bottles).
Optional: Hydrochloric acid or Sulfuric acid.
Optional: pH indicator strips or pH meter.

26
Oil in Soil Extraction Materials

Plastic air syringe with filter frit and plunger (or equivalent).
40 ml vials with Teflon-faced caps.
Analytical balance that reads to 0.100 gram.

Measuring Oil in Water Samples

Extraction Method
1. Collect a known volume of sample between 100 ml and 250 ml in a glass bottle large enough
to add the required amount of solvent - see below:
For example, when doing a 10:1 extraction using the 177 ml prescription bottle provided in
the sampling kit, it is convenient to collect 140 ml of sample and add 14 ml of solvent.
2. For measurements below 200 ppm, calculate 10 percent of the sample volume and add
that volume of solvent.
For measurements above 200 ppm, add the same volume of solvent as there is sample.
3. Replace the cap on the bottle with a septum cap. The sample may be transferred to a
separatory funnel for easier separation. If the sample is transferred to a separatory funnel,
rinse the interior surface and cap of the sample bottle.

If the sample is not to be measured within four hours of sample collection, adjust
the pH to less than 2 with Hydrochloric or Sulfuric acid (typically 3-5 drops
depending on buffers in the sample) and refrigerate at 0 oC - 4 oC.
Warm the sample to room temperature before you continue the sample extraction
process.

4. Shake the bottle or separatory funnel vigorously for 2 minutes with periodic venting to
release excess pressure.

27
 5. Allow the phases to separate. If an emulsion forms similar to this example, see Emulsion
Breaking Techniques on page 39 for detailed instructions.

6. Place a filter paper in the filter funnel.

• For a TOG/FOG measurement, add approximately 1 gram (1 tablespoon) of sodium
sulfate. If the solvent layer is clear, you may skip this step.
• For a TPH measurement, add approximately 1 gram (1 tablespoon) of silica gel.
7. Separate the solvent from the water.

Separating Solvents Heavier than Water

The extract must be either capped or measured immediately.

If you are using the sample bottle method,

1. Withdraw a portion of the solvent (top) layer and deliver through the sodium sulfate/silica
gel into a waste container.
2. Withdraw a portion of the solvent (top) layer and deliver through the sodium sulfate/silica
gel into a clean container. This portion is ready to be analyzed.
If you are using a separatory funnel,
1. Drain the water (bottom) layer along with approximately 1 mL of the solvent layer from
the separatory funnel into a waste bottle.
2. Drain a portion of the solvent layer through the sodium sulfate/silica gel into a waste
container.
3. Drain a portion of thesolvent layer through the sodium sulfate/silica gel into a clean
container. This portion is ready to be analyzed.
Scroll down to Cleaning the Cuvette on page 29 to continue.

Measuring Oil in Soil Samples

Extraction Method
1. Collect a soil sample directly in a washed and weighed (to the nearest 0.100 gram)
EPA/VOA 40 ml vial. The sample should fill about half of the volume of the vial.

28
 2. Weigh the sample to the nearest 0.100 gram, subtracting the tare weight of the vial (the
weight of an empty vial). Note the weight.
3. If the sample is wet and clumpy, add up to 5 grams of silica gel. Use the spatula to break up
the clumps.
4. Add the same volume of solvent in ml as the soil sample weight in grams (do not include the
weight of the silica gel). For example, to 11 grams of soil, add 11 ml of solvent. This will give
a 1:1 extraction ratio.
5. Cap the vial with the Teflon side of the liner toward the sample. Shake the sample vigorously
for 2 minutes.
6. Pour the solvent into the plastic air syringe with filter frit, leaving as much of the soil in the vial
as possible.
7. Place a filter paper in a filter funnel and add approximately 1 teaspoon of silica gel.
8. Depress the air syringe plunger and force the solvent through the filter frit and silica gel into a
clean container.

The extract must be either capped or measured immediately.

9. Clean the cuvette as described in the next section.

Cleaning the Cuvette

1. Fill the cuvette with clean solvent by either pouring directly from the bottle or using a clean
glass pipette.
If measuring samples below 10 ppm, it is recommended to use a clean glass syringe with a
particle filter attached when filling the cuvette with clean solvent in order to remove any dust.
2. Empty contents of the cuvette.
3. Repeat steps 1 and 2.

Zeroing the Analyzer

Before zeroing, the instrument needs to be powered up for a minimum of 30

minutes (longer if stored in a non-temperature-controlled room).

The frequency for zeroing depends on the required sensitivity. For levels below 10 ppm, the
analyzer should be zeroed prior to each measurement and should use the same cuvette for zeroing
and measuring a sample.
For levels 10 ppm and above, zero the analyzer every hour.
1. Fill the cuvette with clean solvent by either pouring directly from the bottle or using a clean,
glass pipette. If measuring samples below 10 ppm, it is recommended to use a clean, glass
syringe with a particle filter attached when filling the cuvette with clean solvent in order to
remove any dust.
2. Cap the cuvette immediately.

29
 3. Clean the clear sides of the cuvette by applying clean solvent and gently wiping dry with a
Kimwipe.
4. Place the cuvette into the instrument; the frosted sides should face forward.
5. From the Main Menu, tap the Zero button to open the following screen:

6. When the measurement timer expires, a result will be displayed on the screen similar to
this example:

7. If the measurement is still not approximately 0, you can consider the ATR crystal clean.
Tap the Set Zero button to force a 0 result and then tap the Done button.

Analyzing a Sample

Before zeroing, the instrument needs to be powered up for a minimum of 30

minutes (longer if stored in a non-temperature-controlled room).

1. Fill the cuvette with the extract approximately halfway up by using a clean syringe or a
clean glass pipette. Cap the cuvette.
2. Shake the cuvette for 5 seconds and then empty out the contents.
3. Using a clean syringe or a clean glass pipette, fill the cuvette at least ¾ of the way with the
extract. Cap the cuvette.
4. Clean the clear sides of the cuvette by applying clean solvent and gently wiping it dry with
a Kimwipe.
5. Place the cuvette into the instrument; the frosted sides should face forward.

30
 6. From the Main Menu, tap the Run button. The following screen opens

Countdown Timer - This is set as part of the configuration and represents the time that must
elapse before the actual sample measurement begins.
Measuring Timer - This displays the sample measurement progress as a percentage.
Single/Continuous Radio Buttons - Tap Single if you just want one measurement pass for the
sample. Tap Continuous if you want the sample to be continuously measured and the result
updated in the Main Menu until you cancel.

Whichever mode you select, all your tests will stay in the same mode until you
select the other radio button.
If you reboot the device, then it will default to Single measurements until you select
Continuous.

Interval Radio Button - Tap one of these radio buttons if you selected the Continuous option, as it
sets the interval between each measurement, either 1, 10, 30 or 60 seconds.
Escape Button - Tap to abort the measurement and return to the Main Menu.
7. The result will appear on the screen once the measurement is finished similar to this
example.

If you chose Continuous the result will be updated depending on the measurement
interval you selected. Be aware that the measurement results may not vary much
from measurement to measurement.
Updates will continue until you stop the process.

31
Results above the Maximum Range or below the Minimum Range as defined in
the configuration you are using will appear in red. If this happens you have two
options:
• Dilute the sample as described in Diluting a Sample on page 41 and retest.
• Create a custom calibration; see Creating a Calibration on page 19 for
details.

32
 7 Accessing Diagnostic Screens
This section describes the following.
Device Information Screen on page 33
Hardware Information Screen on page 33
Hardware Diagnostics Screen on page 34
Power Level Detector Signals Screen on page 34
If you ever need to contact Spectro Support Services, there are screens that you can access that
will provide information likely to be useful to your support engineer, such as software versions, run-
ning voltage and temperature, and detector signal levels. Not all of these screens are accessible to
all user levels.

Make sure no cuvette is present in the sample holder before collecting diagnostic
information.

Device Information Screen

1. From the Main Menu, tap the Zero button.
2. Tap the Info button to open a Device Information Screen similar to this example:

Optional - Tap Done to return to the Zero Menu and tap Done again to return to the Main Menu.
Optional - Tap More to open the Hardware Information Screen.

Hardware Information Screen

1. From the Main Menu, tap the Zero button.
2. Tap the Info button to open the Device Information Screen.

33
 3. From the Device Information Screen, tap the More button to open a Hardware
Information Screen similar to this example:

Optional - Tap Done to return to the Zero Menu and tap Done again to return to the Main Menu.
Optional - Tap Next to open the Hardware Diagnostics Screen.

Hardware Diagnostics Screen

1. From the Main Menu, tap the Zero button.
2. Tap the Info button to open the Device Information Screen.
3. From the Device Information Screen, tap the More button to open the Hardware
Information Screen.
4. From the Hardware Information Screen, tap Next to open the Hardware Diagnostics
Screen similar to this example:

Supply 1 - should be approximately 0.5 V higher than Supply 2.

Current - should be approximately 0.1 A
Power - should be 0.610 W +/-0.05 W.
5. Tap Done to return to the Zero Menu and tap Done again to return to the Main Menu.

Power Level Detector Signals Screen

1. From the Main Menu, tap the Zero button.
2. Tap the Details button to open a Power Level Detector Signals screen similar to this
example:

34
 The detector signal in this example is at 91.1%. If the signal drops below the Alarm level -
60% in this example - contact Spectro Support Services.

3. Tap Done to return to the Zero Menu and tap Done again to return to the Main Menu.

35
 A Correlation to Alternate Method
It may be possible to adjust the calibration so that it correlates better with an alternative method.
In order for this to be possible, the analyzer should be either always reading higher or always
reading lower than the alternative method.
Also, the calibration adjustment will be more effective if the results are off by about the same
factor across the range of the calibration. Use the following procedure for adjusting the cal-
ibration:
1. Measure at least 3 samples and add all the results together.

The samples should be no higher than 90% of the calibration range and no
lower than 10% of the calibration range.

For example:
Sample A = 4
Sample B = 8
Sample C = 16
Total = 28
2. Measure the same exact samples by the alternative method and add all the results
together.
For example:
Sample A = 5
Sample B = 10
Sample C = 20
Total = 35
3. Divide the total from the alternative method by the total from the analyzer:
35/28=1.25
4. Enter this result into the Scale Factor column of the Calibration table.

36
 B Calibration Standard Preparation
This section describes how to make your own calibration standards.

Required Materials
• 125 mL Teflon wash bottle
• 10 mL and/or 20 mL volumetric flasks
• Calibrated glass pipettes in the 0.5-3 mL range (depending on desired stock solution
dilutions)
• Solvent
• Calibration oil
• Analytical Balance that reads to 0.001 gram

Preparing a Stock Solution

Prepare a stock solution and make the appropriate dilutions to cover analysis range. For water ana-
lysis with an extraction ratio of 10:1, the oil and grease is concentrated 10 times in the solvent. The
actual value of the standard is divided by 10 in order to match the concentrated value of the extract.
1. Clean all glassware to be used.
2. Weigh 0.100 gram of oil in a 10 mL volumetric flask.
3. Record the exact weight.
4. Fill with solvent up to the 10 mL line.
5. Place the stopper in the volumetric flask and shake for at least 1 minute.
6. Use the following equation to determine the concentration of stock solution:
C=W/V*1000000
Where:
C = Concentration of Stock Solution (mg/L or ppm)
W = Weight of oil (g)
V = Volume of volumetric flask (mL)

For oil in water or oil in soil calibration using a 1:1 extraction ratio, skip Step 7.

7. For oil in water calibrations using a 10:1 extraction ratio, divide the concentration of the stock
solution by 10 in order to account for the extraction ratio.

37
Preparing Calibration Standards
1. Clean all glassware to be used.
2. For each standard, take a calibrated glass pipette and pipette the stock solution into a 10
or 20 mL volumetric flask and fill with solvent.
3. Place the stopper in the volumetric flask and shake for at least 1 minute.
Using the example of a 1000 mg/L stock solution, dilutions could be as follows:

38
 C Emulsion Breaking Techniques
Certain types of samples, such as those containing detergent, may form emulsions when doing an
oil in water extraction into a solvent. The boundary between the solvent and the sample will have an
emulsion layer that has a cloudy or milky appearance.

According to U.S. EPA Method 1664, “If the emulsion is greater than one-third the volume of the
solvent layer, the laboratory must employ emulsion-breaking techniques to complete the phase
separation."
This is relevant to all oil-in-water measurements that use liquid-liquid extraction whether the
analysis is done by infrared, gravimetric or UV.
If such an emulsion cannot be broken by any attempted means, the test method may not give
representative results for the problem sample. The best way to break or reduce the emulsion
depends on the sample matrix.
The following list includes some options that may be useful for reducing the emulsion enough to be
able to take a valid measurement. All methods are usable with portable infrared analyzers, such as
the InfraCal TOG/TPH analyzers, for virtually any type of oil-in-water measurements, including fat,
oil and grease (FOG) waste-water discharges.
1. Let the sample sit - The easiest is to allow the sample to sit for up to an hour and see if the
emulsion decreases. Make sure the sample is covered to reduce any evaporation of the
solvent. Gently tapping the side of the container or stirring the solvent and emulsion layer
with a stir bar can help to speed up the separation.
2. Centrifuge the sample - A centrifuge is the certain way to break the emulsion but not all labs
and especially on-site facilities have one available.
3. Acidify the sample - If the emulsion is due to an alkali soap, detergent, or surfactant then
lower the pH to 2 with sulfuric acid, (H2SO4) or hydrochloric acid (HCl) (as recommended in
the oil and grease methods, mainly for preservation of the sample). This will modify the
surfactant charge so that is no longer acts as an emulsifier.
4. Add table salt (NaCl)
• If you know that your sample forms emulsions, you can add the salt to the sample with the
solvent and shake the sample.
• If you are trying to break an already formed emulsion, you can shake the salt into the
sample. You should see the salt dropping to the bottom as the droplets from the emulsion
coalesce and the emulsion disappears into cleanly partitioned layers.

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5. If Step 4 is unsuccessful, repeat but use Sodium sulphate instead of salt.
6. If Step 5 is unsuccessful, filter through Sodium sulfate.
• Pipette as much solvent/extract as possible into a clean container without taking the
water layerand add 1 or more grams of anhydrous Sodium sulfate (Na2SO4) and stir with
glass stirring rod. The extract should be non-turbid but may have coloration. Put an 11 cm
No.40 Whatman filter paper into a glass funnel and filter the Sodium sulfate from the
solvent.
Alternately, you may be able to skip the stirring step and just pour the solvent and emul-
sion through the Whatman filter paper with the sodium sulfate. In this case, the sodium
sulfate binds the water leaving the solvent behind so it coalesces into the solvent layer.
7. Ultrasonic bath - Put the solvent/emulsion extract into an ultrasonic bath with ice until the
emulsion is no longer present.

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 D Diluting a Sample
Follow these steps to dilute a sample in a 10:1 ratio.
1. Pour 1 ml of solvent extract into a 10 ml graduated cylinder
2. Add 9 ml of solvent for a 10:1 dilution.
3. Cap the cylinder and shake it thoroughly.
4. Using a 100 μl syringe, add 60 μl of solvent extract to the center of the crystal and tap Run.
5. Add a zero to the result on the display and record your reading, i.e. if the result is 465, the
extract value after dilution is 4,650 ppm.
This procedure may be repeated if the extract is still not measuring within the calibration range. If
you do this, add 2 zeros to the display.
For example, if the result is 465, the extract value after dilution is 46,500 ppm.

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 E InfraCal 2 General Theory of
Operation
The InfraCal 2 is a family of portable infrared (IR) analyzers tailored to provide concentration
values for a specific chemical class in a specific sample material. Each available model is
designed to do the same analysis on every sample that is presented to it.

Infrared Spectra for Analysis of Chemical Functions

The InfraCal 2 uses infrared (IR) energy to determine the concentrations of a target substance.
The instrument focuses on the mid-infrared (mid-IR) region of the electromagnetic spectrum fall-
ing between 2.5 and 25 µm.
When the infrared energy passes into or through a sample, the molecules will begin to vibrate
and cause it to absorb light at specific wavelengths within the mid-IR spectrum. Any IR energy
not absorbed by the sample will be transmitted to the detector.
Various functional groups in the molecules, such as aliphatic hydrocarbon chains, alcohol
groups, or organic acid groups each have specific wavelengths at which they vibrate. By meas-
uring how much of the energy at the specific wavelength of interest has been absorbed by the
sample, the concentration of that chemical class may be determined.
The InfraCal 2 measures the intensity of a specific infrared absorption band in order to determine
the concentration of a sample. The peaks in the graph show where the molecules absorb IR
energy, while the flat spaces along the baseline show IR frequencies where they are transparent.
For example, the TRANS-SP model has an optical filter placed over an infrared detector so that it
can measure light absorbed at 3.4 um. This absorption band is caused by the C-H stretch that is
typical of hydrocarbons and is indicated by the arrow:
Oil and grease hydrocarbons.

Sampling Cell Description

The TRANS-SP model uses a transmission cell to pass the IR energy into the sample.
The TRANS-SPmodel uses a 10 mm Quartz Cuvette for the transmission cell. Quartz is IR-trans-
parent in the region of 3.4 µm, which is a requirement for this analysis.

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 F Specifications

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