Dexsil L2000DXT Manuale utente

Disclaimer

Dexsil Corporation makes no representations or warranties with respect to the contents hereof

and specifically disclaims any implied warranties of merchantability or fitness for any particular

purpose. Further, Dexsil Corporation reserves the right to revise this publication and to make

changes from time to time in the contents hereof without obligation of Dexsil Corporation to

notify any person of such revision or changes.

Trademarks

L2000 and Dexsil are trademarks of Dexsil Corporation.

DEXSIL CORPORATION

One Hamden Park Drive

Hamden, CT 06517

Tel (203) 288-3509

Fax (203) 248-6523

http://www.dexsil.com

Rev. 6, December 2018

Table of Contents

Introduction to the L2000DXT Analyzer .......................................................................2

Sample Preparation.................................................................................................2

Chloride Conversion Reaction................................................................................3

Quantification ........................................................................................................3

Unpacking............ ........................................................................................................4

List of Components.................................................................................................4

List of Reagent Options..........................................................................................5

Option 1 - 40 Oil Tests....................................................................................5

Option 2 - 20 Soil Tests .................................................................................5

Option 2a - 20 Soil Tests (Two-Step Procedure)..............................................5

Option 3 - 20 Water Tests...............................................................................6

Option 4 - 20 Wipe Tests................................................................................6

Initial Set Up........ ........................................................................................................7

Restoring the Electrode After Extended Storage..........................................................7

Basic Operation of the L2000DXT .................................................................................9

General Information......................................................................................................9

Navigating the Operating Program...............................................................................11

Main Menu..... ........................................................................................................11

Calibration...... ........................................................................................................12

Blank Determination...............................................................................................13

Analysis.......... ........................................................................................................15

Entering Header Information..................................................................................16

Creating or Editing a Method .................................................................................16

Data Management...................................................................................................18

Change Date or Time..............................................................................................20

Check Electrode......................................................................................................20

Sample Preparation. ........................................................................................................22

Oil Samples.......... ........................................................................................................22

Soil Samples......... ........................................................................................................22

Standard Procedure for Soil Analysis.....................................................................23

Two-Step Extraction Procedure for Soil Analysis..................................................24

Water Samples..... ........................................................................................................25

High Range (5-2000 ppm)......................................................................................25

Low Range (10 ppb - 5 ppm)..................................................................................25

Wipe Samples ...... ........................................................................................................26

Care and Maintenance .....................................................................................................27

General Care ........ ........................................................................................................27

Electrode Care and Maintenance..................................................................................28

Troubleshooting ....... ........................................................................................................28

Error Messages..... ........................................................................................................30

Appendix A: Additional Information Available from Dexsil .......................................33

Appendix B: Methods Table............................................................................................35

Appendix C: Technical Data............................................................................................37

Appendix D: Program Flow Chart..................................................................................38

Introduction to the L2000DXT Analysis System

Congratulations on your purchase of the L2000DXT Analyzer, a versatile analysis system suitable

for the analysis of a wide variety of chlorinated organic compounds in a variety of matrices. The

basic principal of the L2000DXT system is to measure the total organic chlorine content of a

sample and equate that to an equivalent concentration of the target or expected analyte. If all of

the organic chlorine present is assumed to be derived from the target analyte, then an upper limit

is established for the compound in question. (If other organic chlorines are present, in addition

to the target analyte, they will be counted as the target analyte.) To accomplish this, all of the

organically bound chlorine must be converted into inorganic chloride and the resulting chloride

quantified. Once the total chlorine content of the sample is known, a conversion factor is used to

convert the chloride concentration into an equivalent concentration of the target analyte. If the

contaminant is known, the resulting concentration estimates will accurately correlate with the

actual concentration of the analyte in the sample as determined by confirmatory analysis in the

lab. If the contaminant is unknown, a conservative or worst case conversion factor is chosen to

provide an upper limit for the concentration of the target analyte in the sample.

There are three basic steps involved in the chemical analysis for total halogen by the L2000DXT:

- Sample Preparation

- Conversion to Inorganic Chloride

- Quantification

The sample preparation step determines the type of chlorine detected, i.e., organic, inorganic, or

total, and is matrix dependent. The sample preparation can be as simple as collecting a

transformer oil sample, or can involve the extraction of a soil or water sample. In the case of a

wipe sample, the surface is wiped and the wipe-gauze is extracted. The steps involved in the

conversion to inorganic chloride reaction and the chloride quantification are the same for all

matrices. The steps in the conversion to inorganic chloride involve the reaction of the sample

with metallic sodium and the extraction of the resulting chloride into an aqueous buffer system.

A chloride specific electrode is used to quantify the extracted chloride. Using stored conversion

factors, the chloride value is then converted to an equivalent concentration of analyte.

Sample Preparation

The L2000DXT can be used to analyze the following matrices:

- Transformer Oil

- Soil

- Water

- Surface Wipe

Each matrix requires different preparation prior to the conversion reaction step and subsequent

quantification. Each of the matrix preparation steps are described in detail under Sample

Preparation.

The routine analysis of transformer oil requires no sample preparation other than to collect a

clean sample without introducing any extraneous sources of chloride into the sample, such as

perspiration or road salt. This is important because, for transformer oil, there is no sample

cleanup procedure to remove inorganic chloride contamination. Once collected, the sample is

reacted and the resulting chloride is extracted and quantified.

The chlorine quantified in this case is the total chlorine contained in the sample. Transformer oil

is typically free of inorganic chlorine, eliminating the need for any sample cleanup procedure. In

special cases where transformers have failed due to water contamination or have been removed

for service and stored in areas near seawater or road salt, inorganic chloride may cause an

elevated reading.

Before a soil sample can be analyzed, the organic contaminants must be extracted using an

organic solvent. Because soil samples invariably contain inorganic chlorine, the soil extract is

cleaned up to remove all traces of the inorganic chloride. The cleaned extract is then reacted and

the resulting chloride is quantified. For soil analyses, only the organic chlorine content is ever

quantified. Extraneous sources of chloride contamination such as road salt or sea salt are not

detected.

As with soil samples, a water sample must also be extracted prior to final analysis. The ratio of

the solvent volume to the sample volume determines the sensitivity of the test. The extract is

reacted and the chloride is quantified as above. In water samples, only the organic chlorine is

quantified.

Wipe tests require that a specific area be wiped using a hexane-soaked gauze. The gauze is

extracted with an organic solvent, reacted, and the chlorine content determined. For wipe

samples, the standard procedure eliminates most all inorganic chlorine contamination. Areas

with very high surface concentration of salts may need to be prepared differently.

Chloride Conversion Reaction

Once the sample has been prepared, the remaining chloride conversion steps are the same for all

sample types. The conversion step is a reaction of the sample with an excess of metallic sodium

in the presence of a catalyst to convert the covalently bound organic chlorine into free chloride

ions. This reaction of metallic sodium with organo-chlorine compounds is vigorous and goes to

completion, converting all of the organic chlorine to chloride.

Quantification

Upon the completion of the conversion reaction, the resulting chloride ions are extracted into an

aqueous buffer. The chloride content in the final extract/buffer is then quantified using a

chloride specific electrode and converted to an equivalent analyte concentration using the

conversion factors programmed into the chosen analysis method of the instrument. The

conversion factor is made up of the percent chlorine, the sample size multiplier, and the

extraction efficiency multiplier. The analyte concentration is determined by first subtracting the

blank from the raw chloride reading (except when the Blank Subtraction has been turned off),

and the resulting corrected chloride value is multiplied by the size and extraction multipliers and

divided by the chloride fraction (percent chlorine divided by 100):

[Analyte] = ([Cl-]raw - [Cl-]blank)(size multiplier)(extraction multiplier)/(chlorine fraction)

The L2000DXT Analyzer comes preprogrammed with 33 methods providing for analysis of a

large number of organo-chlorine compounds in most matrices. Correction factors are

preprogrammed to account for all of the steps necessary to run samples using the standard

prepackaged reagents. If the procedures are modified or other analytes are expected, up to 20

custom methods can easily be built.

The operational program of the L2000DXT has been designed to provide the most versatile data

reduction platform possible for the analysis of chlorinated organic compounds in a variety of

matrices. At the same time, the program is easy to use for routine analysis and does not require

custom method development.

Unpacking

The L2000DXT is shipped in its own carrying case, complete with all the hardware necessary for

operation. Upon receiving the L2000DXT Analyzer, please verify that all of the items listed

below are present and in good working order.

The carrying case for the L2000DXT Analyzer should contain the following items:

L2000DXT Electronic PCB/Chloride Analyzer

Power cube AC-DC transformer

Portable electronic balance & 100 g Calibration weight

5 mL pipettor

Vial rack

Timer

Marking pen

USB thumb drive

Two empty 20 mL glass vials for RINSE and CALIBRATION solutions

User’s Manual, Certificate of Calibration and MSDS

NOTE: DO NOT return meter to case with USB Drive installed.

In addition to the aforementioned items in the carrying case, the following should be included in

the same outer shipping box:

Chloride-ion specific electrode1

Packet of polishing strips1

Test tube rack

To prevent damage to the instrument in the case of a leak, the sample preparation reagents are

shipped separately. The exact makeup of the reagent pack will depend on the specific reagent

1These items are shipped in their original packaging from Orion. Once they have been unpacked, they should be carried in the right-hand slot in

option chosen at the time of ordering. The options available for the L2000DXT and the

components contained in each are the following:

Option 1: Reagents for 40 Oil Test

1 - 250 mL bottle of EXTRACT solution

1 - 250 mL bottle of RINSE solution

1 - 250 mL bottle of CALIBRATION solution

1 - 60 mL bottle of Electrode Filling Solution

1 - tray of 40 empty 20 mL glass vials

1 - box of tissue wipes

1 - shelf-pack containing (in a heat sealed foil bag):

40 - filters

40 - pipettes

40 - reaction tubes (black dispenser caps)

Reorder Part No: (LP-ORK)

Option 2: Reagents for 20 Soil Tests (Standard Procedure)

1 - 250 mL bottle of EXTRACT solution

1 - 250 mL bottle of RINSE solution

1 - 250 mL bottle of CALIBRATION solution

1 - 60 mL bottle of Electrode Filling Solution

1 - box of tissue wipes

1 - 40-cell box containing:

20 - empty 20 mL glass vials

20 - bottles containing Soil Extraction Solvent

1 - shelf-pack containing (in a heat sealed foil bag):

20 - filters

20 - pipettes

20 - reaction tubes (black dispenser caps)

20 - metal scoops for obtaining soil samples

20 - 10 mL plastic syringes

20 - drying columns (foil packed)

20 - empty test tubes with white caps

Reorder Part No: (LP-SRK)

Option 2a: Reagents for 20 Soil Tests (Two-Step Extraction Procedure)

1 - 250 mL bottle of EXTRACT solution

1 - 250 mL bottle of RINSE solution

1 - 250 mL bottle of CALIBRATION solution

1 - 60 mL bottle of Electrode Filling Solution

1 - box of tissue wipes

1 - set of instructions

1 - 40-cell box containing:

20 - empty 20 mL glass vials

20 - 6 mL black-capped water vials

1 - shelf-pack containing (in a heat sealed foil bag):

20 - empty 25 mL soil tubes

20 - filter funnels

20 - pipettes

20 - reaction tubes with black dispenser caps

20 - break-top vials containing Soil Extraction Solvent

20 - metal scoops for obtaining soil samples

20 - syringe filters (in a heat sealed foil bag)

1 - set of instructions

Reorder Part No: (LP-SR2)

Option 3: Reagents for 20 Water Tests

1 - 250 mL bottle of EXTRACT solution

1 - 250 mL bottle of RINSE solution

1 - 250 mL bottle of CALIBRATION solution

1 - 60 mL bottle of Electrode Filling Solution

1 - box of laboratory wipes

1 - 40-cell box containing:

20 - empty 20 mL glass vials

20 - bottles of Isooctane

1 - shelf-pack containing (in a heat sealed foil bag):

20 - filters

20 - pipettes

20 - reaction tubes (black dispenser caps)

20 empty test tubes with white caps

1 - set of instructions

Reorder Part No: (LP-WRK)

Option 4: Reagents for 20 Wipe Tests

1 - 250 mL bottle of EXTRACT solution

1 - 250 mL bottle of RINSE solution

1 - 250 mL bottle of CALIBRATION solution

1 - 60 mL bottle of Electrode Filling Solution

1 - box of tissue wipes

2 - pair of safety goggles (1 pair/10 tests)

2 - pair of neoprene gloves (1 pair/10 tests)

1 - shelf-pack containing (in a heat sealed foil bag):

20 - filters

20 - pipettes

20 - reaction tubes (black dispenser caps)

20 - hexane ampules

20 - empty test tubes with white dispensing caps

1 - box containing:

20 - gauze pads in 20 mL glass vials

20 - 10 mL glass bottles containing Extraction Solvent (isooctane)

1 - box containing:

20 - empty 20 mL glass vials

20 - forceps

1 - set of instructions

Reorder Part No: (LP-WIP)

NOTE: DO NOT STORE REAGENTS IN THE INSTRUMENT CARRYING CASE, AS ANY

LEAKS WILL DAMAGE THE INSTRUMENT.

Initial Set Up

Once the L2000DXT has been unpacked, the components checked and the contents of the reagent

pack verified, the L2000DXT can be set up for analysis. Locate the vial rack, the two empty 20

mL vials and the bottles of RINSE and CALIBRATION solutions. Remove the caps from both

vials and label one 20 mL vial “RINSE” and the other “CAL”. Fill each vial approximately ½

full with the appropriate solution and set in vial rack. (NOTE: It is helpful to label the rack with

the location of the RINSE and CAL vials.) These solutions will be used for the initial setup and

calibration of the electrode. They will also be used periodically to re-calibrate the electrode and

check the electrode output. Once set up, the electrode should remain in the RINSE solution

when not in use.

Prior to running the Analyzer on battery power, it should be charged overnight using the power

cube supplied with the instrument. The Analyzer can be operated from line power while the

battery is charging and should be left plugged in whenever AC power is available.

WARNING: STATIC ELECTRIC SHOCKS CAN DAMMAGE THE

ELECTRODE AND THE METER. DO NOT ATTACH ELECTRODE

WHEN METER IS ON.

Restoring the Electrode after Extended Storage

The electrode is shipped empty and should be stored empty whenever it will be left for an

extended period of time or placed in the carry case (see Electrode Care and Maintenance).

To restore the electrode to operating condition:

1. Remove protective cap from the tip of the electrode.

2. Fill the electrode, up to the filling hole in the side, with the Orion Electrode Filling

Solution supplied with each lot of reagents. To fill, place the nozzle of the fill

solution bottle into the hole on the side of the plastic body and gently squeeze the fill

bottle.

3. Drain the electrode, while holding it upright over the waste beaker, by grasping the

body of the electrode firmly in one hand and pushing down on the black cap where

the cord enters the electrode. The filling solution will drain out of the bottom of the

electrode.

4. Refill the electrode and make sure that the fill solution is making contact between the

black cone and the plastic shell at the bottom of the electrode. If it is not making

contact at all points, drain the electrode again and refill.

5. With the meter off, connect the electrode to the BNC connector labeled “Electrode”

on the back of the L2000DXT Analyzer and check electrode output.

6. To check the electrode, turn the Analyzer on by pressing the ON Button on the back

panel of the instrument. From the START SCREEN press ENTER to open the

MAIN MENU. At the MAIN MENU, press DIAG to open the DIAGNOSTICS

screen. This display:

will indicate the current system information and then continuously update the

electrode output in millivolts (mV). Place the electrode in fresh RINSE solution,

gently swirl the solution with the electrode and allow to equilibrate. The electrode

output should reach 140 mV or greater within 1 minute. If the electrode output does

not reach at least 140 mV by the time the 2 minute buzzer sounds, empty the RINSE

solution and refill with fresh RINSE solution. If this does not improve the electrode

output, drain the electrode, refill it with filling solution and check the output again.

NOTE: When setting up the L2000DXT after the unit and/or electrode has been in

storage or is brought from a colder/warmer environment, it is important to allow both

the unit and the electrode to equilibrate for as long as possible. It could take up to an

hour for the electrode to equilibrate. Once the output is greater than 140 mV, the

electrode is functioning correctly and it is safe to proceed with measurements. If the

electrode output does not reach 140 mV, see under Troubleshooting for remedies.

NOTE: The update rate for the DIAGNOSTICS screen is 10-20 seconds, any keys pressed will

not register until the end of the current measurement cycle. Therefore, to exit the

DIAGNOSTICS screen, the BACK button must be pressed until the meter registers the input.

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