Spectro Scientific InfraCal 2 ATR-SP User Manual
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Spectro Scientific InfraCal 2 ATR-SP User Manual

Measuring oil and grease from water and soil
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InfraCal 2 ATR-SP User's Guide
Measuring Oil and Grease from Water and Soil
Doc p/n 100-00316
|
Rev. C
February 2019
Spectro Scientific - An ISO 9001:2015 Company
One Executive Drive, Suite 101, Chelmsford, MA 01824 Tel. (+1) 978-431-1120
www.spectrosci.com
Sales@spectrosci.com
Support@spectrosci.com

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  • Page 1 InfraCal 2 ATR-SP User's Guide Measuring Oil and Grease from Water and Soil Doc p/n 100-00316 Rev. C February 2019 Spectro Scientific - An ISO 9001:2015 Company One Executive Drive, Suite 101, Chelmsford, MA 01824 Tel. (+1) 978-431-1120 www.spectrosci.com Sales@spectrosci.com Support@spectrosci.com...

  • Page 2: Spectro Scientific Warranty

    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:...

  • Page 3: Spectro Scientific Phone Numbers

    (3) refund the purchase price of the product. 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...

  • Page 4: Safety Information

    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.

  • Page 5: Definitions

    Title to, ownership of and all patent, copyright, trade secrets and other intellectual property rights in the Unit, Software or any of it parts shall at all times remain with SPECTRO SCIENTIFIC. Software is confidential and proprietary and Licensee shall observe the proprietary nature thereof.

  • Page 6: 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.

  • Page 7: Miscellaneous

    Agreement shall be only in Boston, Massachusetts, USA, provided that SPECTRO SCIENTIFIC may seek equitable relief in any court of competent jurisdiction. This Agreement states the entire understanding between the parties as to Software licensed here- under.

  • Page 8: Table Of Contents

    Table of Contents Copyright Notice Spectro Scientific Warranty Spectro Scientific Phone Numbers Spectro Scientific Trademarks Spectro Scientific Patents U.S. Other Countries Document Conventions Safety Information Personal Precautions Environmental Precautions Document Revision History 1. Definitions 2. Scope of Authorized Use 3. Title and Ownership: Confidentiality 4.
  • Page 9 4 Administrative Functions Adding a Security PIN to the Default Admin Changing Users Adding a New User Editing Existing Users Deleting Users Adding Data Labels Selecting a Calibration Editing a Calibration Deleting a Calibration Reviewing Saved Measurements Exporting Saved Measurements Deleting Saved Measurements Updating the Software 5 Creating a Calibration...
  • Page 10 D InfraCal 2 General Theory of Operation Infrared Spectra for Analysis of Chemical Functions Sampling Cell Description Quantitative Analysis E Diluting a Sample F Specifications...

  • Page 11: Introduction

    InfraCal 2 General Theory of Operation on page 41. The InfraCal 2 ATR-SP analyzer is designed to measure solvent extractable material (oil and grease) by infrared determination in water or soil using hexane, pentane, cyclohexane or Vertrel MCA for the extraction procedure. A detector with a fixed 3.4 µm (2940 cm ) filter is used to measure oil and grease concentrations.

  • Page 12: Quick Reference Guide

    Quick Reference Guide This section assumes you have prior training or experience with the device. Allow the device to warm-up for at least 30 minutes. Level the device using the bubble level on top. If you have any custom calibrations, tap Analysis and select a calibration from the table and tap Done.

  • Page 13: Getting Started

    Unpacking the Shipping Carton Unpack the shipping carton and compare the contents with the packing list. If they do not match, contact Spectro Scientific immediately. Installation Location The instrument is designed for on-site measurements and is relatively insensitive to vibration and ambient temperature changes.

  • Page 14: Activating The Internal Battery

    Activating the Internal Battery 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. The battery will not begin to charge until after the first time you power the device up using the charger/adapter with the slide switch on the bottom of the analyzer set to ON.

  • Page 15: Touch Screen Interface Description

    Connect the AC side of the power supply to the utility power connector or other appropriate AC power source. Push the power button on the back of the device to boot the device to the Main Menu. To power down, press and hold the power button until the screen turns off. No settings will be lost.
  • Page 16 2. Units of Measure - Depends on the device type. Examples may include ppm, mg/l or mg/kg. Tap the units to switch between Concentration Units and Absorbance. 3. Test Result - Displays the test result to the number of decimal places specified in the calibration.

  • Page 17: Navigating Tables

    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: Navigating Tables...

  • Page 18: Setting The User Interface Language

    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.

  • Page 19: Setting Battery Stretch And Display Brightness

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

  • Page 20: Administrative Functions

    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...

  • Page 21: Changing Users

    From the Security Menu, tap the Admin user entry to highlight it: Underneath the list of users is the PIN Required option. Tap the blue Admin radio button to select it: Tap the Edit button, then tap in the PIN field: A calculator-style keypad opens.

  • Page 22: Adding A New User

    Tap the down arrow next to the User Name field and select the user you want to change to: 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. From the Main Menu, tap the Setup button.

  • Page 23: Editing Existing Users

    Create a PIN (minimum of 4 digits) and press = to enter. 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. 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.

  • Page 24: Selecting A Calibration

    Tap the Data button to open the Label screen: Tap inside the white box for Label 1 to open a keyboard to add a descriptive label: Optional: Tap the Label 2 field to add a second label. Tap the Done button. Selecting a Calibration Your instrument may ship with a factory calibration.

  • Page 25: Editing A Calibration

    Editing a Calibration You must be logged in as an Admin-level user. Tap the Analysis button. Tap the calibration to be edited. • If the middle button says Edit, any Admin user can edit all settings for any Custom calibration •...

  • Page 26: Exporting Saved Measurements

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

  • Page 27: Deleting Saved Measurements

    • 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): 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.

  • Page 28: Updating The Software

    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. 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.
  • Page 29 When the device detects the new software, tap the Software button to start a series of compatibility checks. Once the checks are complete, tap Update and then confirm; this will install the new software.

  • Page 30: Creating A Calibration

    Creating a Calibration You must be logged in as an Admin-level user. From the Main Menu, tap the Analysis button to open the Analysis Menu. 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.
  • Page 31 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. Tap Next to open the following menu: Analytical: Not accessible - default only.
  • Page 32 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 Absorb- ance and Concentration values for each calibration standard to continue with this section.

  • Page 33: Measuring Calibration Standards

    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: We recommend you begin with the lowest concentration standard and work up.
  • Page 34 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: Clean the crystal 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.

  • Page 35: Graphing The Calibration Points

    Optional: Tap the Graph icon to display the table entries as a graph. See Graphing the below for details. Cal-ibration Points 10. 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.

  • Page 36: Testing Samples With The Atr-Sp

    Testing Samples With the ATR-SP This section describes the following: Solvents on page 26 Sample Extraction Materials on page 26 Measuring Oil in Water Samples on page 28 Measuring Oil in Soil Samples on page 29 Cleaning the ATR Crystal on page 30 Zeroing the Analyzer on page 30 Analyzing a Sample...

  • Page 37: Oil In Water Extraction Materials

    Oil in Water Extraction Materials • 125 mL Teflon wash bottle • 100 mL stopper graduated cylinder or sample bottles (for solvents lighter than water) • 125 mL stoppered separatory funnel or sample bottles with septa caps (for solvents heavier than water) •...

  • Page 38: Measuring Oil In Water Samples

    Measuring Oil in Water Samples Extraction Method 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.

  • Page 39: Separating Solvents Heavier Than Water

    Separating Solvents Heavier than Water The extract must be either capped or measured immediately. • If you are using the sample bottle method, invert the bottle so that the solvent layer fills the neck. Using a 5 ml syringe, withdraw 4 - 5 ml of the solvent (bottom) layer and deliver through the sodium sulfate/silica gel into a clean container.

  • Page 40: Cleaning The Atr Crystal

    Place a filter paper in a filter funnel and add approximately 1 teaspoon of silica gel. 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 after extraction. Continue to the next section: Cleaning the ATR Crystal.

  • Page 41: Analyzing A Sample

    From the Main Menu, tap the Zero button to open the following screen: If you skipped Step 2, and your crystal is dry, there is no need to wait for the countdown to finish because there are no solvents to evaporate off the crystal. Tap the Skip button and the Zero measurement timer will start.
  • Page 42 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.

  • Page 43: Conducting A Solvent Purity Test

    Conducting a Solvent Purity Test For measurements below 10 ppm, solvent purity testing is a requirement. For measurements 10 ppm or greater we recommend that you check solvent purity periodically based on throughput. If you have more than 1 calibration configured on your device, open the Analysis menu and select the calibration to be used for the sample measurement and press Done.

  • Page 44: Accessing Diagnostic Screens

    Accessing Diagnostic Screens 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, running voltage and temperature, and detector signal levels. Not all of these screens are accessible to all user levels.

  • Page 45: Hardware Diagnostics Screen

    Hardware Diagnostics Screen From the Main Menu, tap the Zero button. Tap the Info button to open the Device Information Screen. From the Device Information Screen, tap the More button to open the Hardware Information Screen. 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.

  • Page 46: A Correlation To Alternate Method

    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.

  • Page 47: B Calibration Standard Preparation

    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) •...

  • Page 48: Preparing Calibration Standards

    Preparing Calibration Standards Clean all glassware to be used. 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. 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:...

  • Page 49: C Emulsion Breaking Techniques

    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.
  • Page 50 • 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. If Step 4 is unsuccessful, repeat but use Sodium sulphate instead of salt.
  • Page 51 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.
  • Page 52 Sampling Cell Description The ATR model uses an HATR (Horizontal Attenuated Total Reflectance) crystal to pass the IR energy into the sample. The ATR models use a Cubic Zirconia (CZ) crystal for the attenuated total reflectance cell. It has a refractive index higher than any of the sample materials that are analyzed with the InfraCal, which is a requirement for an ATR material.
  • Page 53 The diagram below shows the phenomenon of ATR. The d in the exploded view (top part in red) shows the tiny portion of a wave that protrudes into the sample before returning to the crystal: Quantitative Analysis In order to obtain accurate quantitative values from the InfraCal 2, values obtained from unknown samples are compared to a calibration curve gathered from standards of known concentrations.
  • Page 54 Diluting a Sample Follow these steps to dilute a sample in a 10:1 ratio. Pour 1 ml of solvent extract into a 10 ml graduated cylinder Add 9 ml of solvent for a 10:1 dilution. Cap the cylinder and shake it thoroughly. Using a 100 μl syringe, add 60 μl of solvent extract to the center of the crystal and tap Run.
  • Page 55 Specifications Type Fixed filter infrared analyzer Dimensions 17 x 19.8 x 13.2 cm (6.7 x 7.8 x 5.2” ) Weight 2.6 kg (5.8 lbs) 0.5A @ 18 VDC input Power Requirements 2.1A @ 18 VDC input with battery charging Power supply (P/N: 200-00306) Input: 100 - 250 VAC, 50/60 Hz Power Source Output: 18 VDC, 3.3 A max.

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