QuickTrace M-6100 Mercury Analyzer Operator Manual

Version 1.0.1

Part Number: 480120

 by anyone other than by CETAC
Product Warranty authorized personnel or agents
will void this warranty. If any
Statement
non-CETAC component is
SD Acquisition, Inc., DBA installed in the CETAC
CETAC Technologies manufactured unit without the
(“CETAC”), warrants any approval of CETAC, the
CETAC unit manufactured or warranty will be voided. In
supplied by CETAC for a period addition, this warranty does not
beginning on the date of extend to repairs made necessary
shipment and ending on the by the use of parts, accessories
sooner to occur of: (a) the date or fluids which are either
that is twelve (12) months from incompatible with the unit or
the date of installation, or (b) the adversely affect its operation,
date that is thirteen (13) months performance or durability.
from the date of shipment. Units CETAC’S obligation under this
found in the reasonable warranty is strictly and
judgement of CETAC to be exclusively limited to repair or
defective in material or replacement of defective
workmanship will be repaired or CETAC parts, and no claim of
replaced by CETAC without breach of warranty shall be
charge for parts and labor. cause for cancellation or
CETAC reserves the right to recission of the contract of sale
change or improve the design of of any unit.
any unit without assuming any
obligation to modify any unit The foregoing express warranty
previously manufactured. is in lieu of all other warranties,
expressed or implied, including
This warranty does not cover warranties of merchantability
any unit that has been subject to and fitness for a particular
misuse, neglect, negligence, or purpose. CETAC shall not be
accident. The warranty does not bound by any representations or
apply to any damage to the unit statements on the part of its
that is the result of improper employees or agents whether
installation or maintenance, or to oral or in writing and including
any unit that has been operated any made in catalogues and
or maintained in any way other promotional material
contrary to the instructions including technical details and
specified in the CETAC specifications except where such
instruction and operation representations and statements
manual. Operation of the are expressly made part of this
CETAC unit inside a laboratory contract. CETAC assumes no
fume hood with stagnant air is responsibility for incidental,
contra-indicated and will void consequential or other damages,
the warranty. Any attempt to even if advised of such a
repair or alter any CETAC unit

iii
possibility, including but not
limited to loss or damage of
property, loss of revenue, loss of
use of the unit, loss of time, or
inconvenience. CETAC’s
liability on any claim for loss or
damage arising out of the sale,
resale or use of any of its
products shall in no event
exceed the selling price of the
unit.

iv
 Products may not be returned
Purchaser shall indemnify which are contaminated by
CETAC against any claim or radioactive materials, infectious
liability which may be asserted agents, or other materials
as relates to the following: (i) the constituting health hazards to
use to which any product CETAC employees.
supplied hereunder is put
infringes the patent, copyright or
other intellectual property rights Returned Product
of any third party; or (ii) any
liability resulting from the
Warranty
failure by Purchaser to observe Determination
the terms of this Warranty. After CETAC’S examination,
warranty or out of warranty
status will be determined. If a
Returned Product warranted defect exists, the
Procedures product will be repaired at no
charge and shipped prepaid back
Claims for shipment damage to the buyer. If the buyer desires
(evident or concealed) must be an air freight return, the product
filed with the carrier by the will be shipped collect.
buyer. CETAC must be notified Warranty repairs do not extend
within ninety (90) days of the original warranty period.
shipment of incorrect materials.
No product may be returned, If an out of warranty defect
whether in warranty or out of exists, the buyer shall be notified
warranty, without first obtaining of the repair cost. At such time
approval from CETAC. No the buyer must issue a valid
replacements will be provided purchase order to cover the cost
nor repairs made for products of repair and freight, or
returned without such approval. authorize the products to be
Any returned product must be shipped back as is, at the buyer’s
accompanied by a return expense. Failure to obtain a
authorization number. The purchase order number approval
expense of returning the unit to within fifteen (15) days of
CETAC for service will be paid notification will result in the
by the buyer. The status of any products being returned as is, at
product returned later than thirty the buyers expense.
(30) days after issuance of a
return authorization number will
be subject to review. Shipment
of repaired products will
generally be made within 5
working days after they are
received.

v
COPYRIGHT SAFETY
Copyright SD Acquisition, Inc., DBA
CETAC Technologies Instruments, accessories, components or
480120 Version 1.0.1, 2003 other associated materials may not be
returned to CETAC Technologies if
contaminated with biohazard or
REPRODUCTION
radioactive materials, infectious agents, or
any other materials and/or conditions that
All rights reserved. Reproduction or could constitute a health or injury hazard
transmission of this document in whole or to CETAC employees. Call Customer
in part, and by any means without the Service and Support if there is any
express written consent of the copyright question or doubt relative to
owner or authorized agent is prohibited. decontamination requirements.
Requests for additional copies of this, or
any other CETAC publication, can be
CAUTION and WARNING statements, as
filled by contacting an authorized
applied in this document, shall be
distributor or
interpreted consistent with the following
CETAC Technologies context: CAUTION applies only to
Customer Service & Support potential property damage conditions;
14306 Industrial Road WARNING applies to potential personal
Omaha, Nebraska 68144, USA injury conditions, in combination with or
Phone (800) 369-2822 (USA only) exclusive of potential property damage.
Phone (402) 733-2829
Fax (402) 733-1932
E-mail custserv@[Link] WARNING

DISCLOSURE The handling of organomercurial

concentrates which may be used in the
preparation of process standards presents
This document contains CETAC
a substantial (potentially lethal) safety
proprietary data and is provided solely to
hazard. Only an experienced,
its customers for their express benefit of
professionally trained organo-metallic
safe, efficient operation and maintenance
chemist, knowledgeable and skilled
of the product described herein. Use or
specifically in the safe handling of
disclosure of CETAC proprietary data for
organomercurials (using approved
the purpose of manufacture or
apparatus and approved protection
reproduction of the item described herein,
measures in an approved facility) should
or any similar item, is prohibited, and
attempt to prepare diluted
delivery of this document shall not
organomercurial process standards from
constitute any license or implied
concentrates.
authorization to do so.

NOTE
REVISIONS

SD Acquisition, Inc., DBA CETAC

CETAC Technologies strives to provide
Technologies assumes no liability for the
the scientific community with an
handling of organomercurial concentrates
unparalleled combination of effective
or the preparation, handling, or use of
technology and continuing value.
diluted organomercurial process
Modular upgrades for existing
standards. Instead, CETAC Technologies
instruments will continue to be a prime
recommends use of appropriate standard
consideration as designs progress.
reference materials to validate sample
preparation (dissolution/digestion) and
CETAC Technologies reserves the right to use of inorganic mercury standards for
revise this document and/or improve instrument calibration.
products described herein at any time
without notice or obligation. Warranty
All user-serviceable components are
registration entitles the named owner
specifically identified in this document as
exclusively to manual change pages/new
such; the balance shall be assumed to
editions as they are published.
require the expertise of a factory service
technician/engineer for adjustment,
repair, replacement, modification, etc.
Others not so qualified and performing
these actions shall do so at their own risk.
Furthermore, never operate the

vi
 instrument without first reading and
understanding the QuickTrace Mercury
Analyzer Operator Manual and ensuring
that it is operated safely and properly.

ORIGINAL PACKAGING

Retain original factory packaging for

moves and factory return shipments.
Shipping in anything other than the
original fitted foam and container can
result in incidental damage from which
the purchaser will not be protected under
warranty.

Under all conditions the user must observe safe laboratory

WARNING
procedures during the operation of this product.

vii
viii
 Operator’s Manual Addendum
Notices and Compliance Declarations

FEDERAL CANADIAN NOTICE

COMMUNICATIONS
This digital apparatus does not exceed the
COMMISSION (FCC) NOTICE
Class A limits for radio noise emissions
from digital apparatus as set out in the
This equipment has been tested and found interference-causing equipment standard
to comply with the limits for a Class A entitled "Digital Apparatus." ICES-003 of
digital device, pursuant to Part 15 of the the Department of Communications.
FCC Rules. These limits are designed to
provide reasonable protection against
harmful interference in a commercial POWER CORD SET
installation. REQUIREMENTS

This equipment generates, uses, and can The power cord set supplied with your
radiate radio frequency energy and, if not instrument meets the requirements of the
installed and used in accordance with the country where you purchased the
instructions, may cause harmful instrument.
interference to radio communications.
Operation of this equipment in a If you use the instrument in another
residential environment is likely to cause country, you must use a power cord set
harmful interference, in which case the that meets the requirements of that
user will be required to correct the country.
interference at his own expense.
The AC power cord is the power mains
diconnect for this instrument or
MODIFICATIONS accessories.

The FCC requires the user to be notified

that any changes or modifications made to
this device that are not expressly
approved by CETAC Technologies may
void the user's authority to operate the
equipment.

CABLES

Connections to this device must be made

with shielded cables with metallic
RFI/EMI connector hoods to maintain
compliance with FCC Rules and
Regulations.

ix
 Operator’s Manual Addendum
Notices and Compliance Declarations

This equipment is designed for connection to a grounded

WARNING
(-earthed) outlet. The grounding type plug is an important
safety feature. To reduce the risk of electrical shock or damage
to the instrument, do not disable this feature.

WARNING To reduce the risk of fire hazard and electrical shock, do not
expose the unit to rain or humidity. To reduce the risk of
electrical shock, do not open the cabinet. All maintenance is to
be performed by an Authorized CETAC Service Provider.
Protection provided by the equipment may be impaired if the
equipment is used in a manner not specified by the
manufacturer.

CLEANING INSTRUCTIONS

To clean the exterior surfaces of the instrument, complete the following steps:

1. Shut down and unplug the instrument. 3. Repeat step 2, using a towel dampened
with clean water.
2. Wipe the instrument exterior surfaces
only using a towel dampened with a lab- 4. Dry the instrument exterior using a dry
grade-cleaning agent. towel.

Do not allow any liquid to enter the instrument cabinet, or come

WARNING
into contact with any electrical components. The instrument
must be thoroughly dry before you reconnect power, or turn the
instrument on.

COOLING FAN OBSTRUCTION

The instrument cooling fan(s) shall remain unobstructed at all times. Do not operate the
instrument if the cooling fan(s) are blocked or obstructed in any manner.

ENVIRONMENTAL

Operating Temperature: 10° to 30°C

Relative Humidity 0% to 95%
Operating Altitude 0 to 2000 m

Other Compliance Declarations

Over-voltage Category Over voltage category II
Polution Category Polution Category II
Rated Degree of Protection IEC 60529

x
 Operator’s Manual Addendum
Notices and Compliance Declarations

PANNEAU NE DOIT ÊTRE ENLEVE QUE

PAR UN RÉPARATEUR QUALIFIÉ.

AVERTISSEMENT
POUR UNE PROTECTION CONTINUÉ AVERTISSEMENT
CONTRE LES RISQUES D’INCENDIE, TOUT CONTACT AVEC LES HAUTES
REMPLACER UNIQUEMENT PAR DES TENSIONS PEUT ENTRAINER LA MORT
FUSIBLES DE MÊME TYPE ET OU DES BLESSURES SÉVÈRES. CE
AMPÈRAGE. PANNEAU NE DOIT ÊTRE ENLEVE QUE
PAR UN RÉPARATEUR QUALIFIÉ.

AVERTISSEMENT
NE PAS GLISSER LA MAIN SOUS OU DERIERE LES
ECRANS THERMIQUES DU FOUR. GARDER LA
PORTE D'ACCES AU DEVANT DU BOITIER BIEN FERMEE
POUR ASSURER LA PROTECTION CONTRE LES
BRULURES

AVERTISSEMENT
TOUT CONTACT AVEC LES HAUTES
TENSIONS PEUT ENTRAINER LA MORT
OU DES BLESSURES SÉVÈRES. CE
PANNEAU NE DOIT ÊTRE ENLEVE QUE
AVERTISSEMENT PAR UN RÉPARATEUR QUALIFIÉ.
TOUT CONTACT AVEC LES HAUTES
TENSIONS PEUT ENTRAINER LA MORT
OU DES BLESSURES SÉVÈRES. CE

xi
Operator’s Manual Addendum
Notices and Compliance Declarations

Caution (refer to accompanying

documents)

AVERTISSEMENT
POUR LA PROTECTION PERMANENTE
CONTRE UN CHOC ÉLECTRIQUE, UNE
BRÛLURE DES YEUX (RADIATION UV)
OU DE LA PEAU, LAISSER LE
COUVERCLE HERMÉTIQUEMENT FERMÉ
LORSQUE L’APPAREIL EST SOUS
TENSION.
LAISSER REFROIDIR 5 MINUTES
(APPAREIL ÉTEINT) AVANT D’ENLEVER
LE COUVERCLE.
AVERTISSEMENT
TOUT CONTACT AVEC LES HAUTES
TENSIONS PEUT ENTRAINER LA MORT
OU DES BLESSURES SÉVÈRES. CE
PANNEAU NE DOIT ÊTRE ENLEVE QUE
PAR UN RÉPARATEUR QUALIFIÉ.

AVERTISSEMENT
SURFACES CHAUDES, LAISSER LE
COUVERCLE HERMÉTIQUEMENT FERMÉ.
POUR ACCÉDER, METTRE LA
TEMPÉRATURE DU FOUR À ZÉRO,
OUVRIR LE COUVERCLE ET LAISSER
REFROIDIR 5 MINUTES AVANT DE
TOUCHER LA VERRERIE OU TOUTE
SURFACE MÉTALLIQUE INTÉRIEURE.

xii
Contents
Contents

QUICKTRACE M-6100 MERCURY ANALYZER

OPERATOR MANUAL VERSION 1.0.1

PART NUMBER: 480120

PRODUCT WARRANTY STATEMENT .......................................................... III
RETURNED PRODUCT PROCEDURES.......................................................... V
RETURNED PRODUCT WARRANTY DETERMINATION........................... V
NOTICES AND COMPLIANCE DECLARATIONS ....................................................... IX
CONTENTS ......................................................................................................... XIII
0. PREFACE .......................................................................................................XX
0.1 WHO SHOULD READ THIS BOOK......................................................... XX
0.2 HOW TO USE THIS BOOK....................................................................... XX
0.3 CONVENTIONS USED IN THIS BOOK ................................................. XXI
Instructions ...................................................................................................xxi
Menu Items....................................................................................................xxi
Notes .............................................................................................................xxi
Cautions .......................................................................................................xxii
Warnings......................................................................................................xxii
0.4 TERMINOLOGY ...................................................................................... XXII
0.5 WHERE TO GO FOR MORE INFORMATION ...................................... XXII
0.6 LIST OF TABLES AND FIGURES......................................................... XXIII
1. INTRODUCTION ............................................................................................. 2
1.1 OVERVIEW .................................................................................................. 2
1.2 SYSTEM FEATURES .................................................................................. 2
1.3 SYSTEM PERFORMANCE SPECIFICATIONS......................................... 3
2. PREPARING FOR INSTALLATION............................................................. 6
2.1 SUPPLIES ..................................................................................................... 6
2.1.1 Necessary Supplies................................................................................. 6
2.1.2 Recommended Supplies.......................................................................... 8
2.2 CHOOSING A LOCATION.......................................................................... 9
2.3 SPACE REQUIREMENTS ........................................................................... 9
2.4 VENTILATION .......................................................................................... 10

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 QuickTrace Mercury Analyzer Operator’s Manual
Contents

2.5 POWER REQUIREMENTS ........................................................................11

2.6 UNPACKING THE QUICKTRACE M-6100 .............................................12
3. INSTALLING THE QUICKTRACE M-6100 ................................................16
3.1 PLACEMENT OF THE ASX-400 AUTOSAMPLER AND PERISTALTIC
PUMP.................................................................................................................17
3.2 ELECTRICAL CONNECTIONS.................................................................18
3.3 PC INTERFACE ..........................................................................................20
3.4 AUTOSAMPLER AND PERISTALTIC PUMP AUXILIARY CABLES ..20
3.5 INSTALLING THE AUTOSAMPLER Z DRIVE AND SAMPLE PROBE...
............................................................................................................................21
3.6 VERIFYING THE INSTALLATION..........................................................21
3.6.1 Testing the Interface .............................................................................21
3.7 VERIFY THE SOFTWARE CONFIGURATION OF COM PORTS
MANUALLY .....................................................................................................22
3.7.1 Using Windows HyperTerminal Program ............................................22
3.8 CHECKING THE AUTOSAMPLER COMPONENTS ..............................24
3.9 TESTING THE SAMPLE PROBE..............................................................25
3.10 CARRIER GAS CONNECTION ...............................................................25
3.11 MERCURY TRAP (KMNO4) ...................................................................26
3.12 NAFION® DRYER CARTRIDGE............................................................28
3.13 PLUMBING CONNECTIONS ..................................................................30
3.13.1 Installing the Peristaltic Pump Tubing...............................................30
3.13.2 Installing the Mixing Tee and Drain Tees ..........................................31
3.13.3 Connecting the Liquid Mix and Drain Lines ......................................32
3.13.4 Connecting the Reagent sipper tube and Sample Probe ....................33
3.13.5 Connect the ASX-400 Rinse Station Tubing .......................................34
3.13.6 Peristaltic Pump Tubing Clamp Tension............................................37
4. USING THE QUICKTRACE M-6100 ............................................................42
4.1 THEORY OF OPERATION ........................................................................42
4.1.1 ASX-400 Autosampler ..........................................................................42
4.1.2 QuickTrace M-6100 Automated Mercury Analyzer..............................43
[Link] Sample Introduction and Stannous Chloride Reactor................................43
[Link] Gas-Liquid Separation...............................................................................44
[Link] Carrier Gas ................................................................................................45
[Link] Optics and Cold Vapor AAS .....................................................................45
4.2 SOFTWARE ................................................................................................47
4.3 PREPARING REAGENTS AND CALIBRATION STANDARDS ............47
4.4 CARRIER GAS CONTROL................................................................................50

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QuickTrace Mercury Analyzer Operator’s Manual
Contents

4.5 START-UP AND ANALYSIS OF SAMPLES ........................................... 51

4.5.1 Wetting of the GLS ............................................................................... 51
4.6 QUICKTRACE M-6100 STARTUP SUMMARY...................................... 54
TYPICAL RESULTS AND SETTINGS ................................................................... 56
4.7 PLACING THE QUICKTRACE M-6100 IN STANDBY MODE ............. 58
4.8 COLD SHUTDOWN................................................................................... 58
4.9 SUMMARY OF QUICKTRACE M-6100 SHUT DOWN.......................... 59
5. MAINTAINING THE QUICKTRACE M-6100............................................ 62
5.1 DAILY MAINTENANCE (ALWAYS CHECK BEFORE ANALYSIS) ... 62
5.2 WEEKLY MAINTENANCE ...................................................................... 63
5.3 MONTHLY MAINTENANCE ................................................................... 63
5.4 YEARLY MAINTENANCE ....................................................................... 63
5.5 ASX-400 YEARLY MAINTENANCE ....................................................... 64
5.6 REMOVAL OR INSPECTION OF THE SAMPLE CELL......................... 65
5.6.1 Opening the Optics Door ..................................................................... 65
5.6.2 Removing the Sample Cell ................................................................... 66
5.7 CLEANING THE CELL WINDOWS......................................................... 67
5.7.1 Quick Exposed Surface Cleaning......................................................... 67
5.7.2 Dismantling for Total Cleaning ........................................................... 68
5.8 CELL ASSEMBLY ..................................................................................... 69
5.9 CLEANING THE GAS-LIQUID SEPARATOR ........................................ 72
5.10 CHANGING THE EXTERNAL GAS TUBING ...................................... 73
5.11 RETUBING THE GAS-LIQUID SEPARATOR ...................................... 76
5.11.1 GLS Inlet ............................................................................................ 76
5.11.2 GLS Drain.......................................................................................... 77
5.13 REPLACING THE NAFION® DRYER CARTRIDGE ........................... 78
5.14 GLS OVERFLOW RECOVERY .............................................................. 79
5.15 REPLACING THE HG LAMP BULB ...................................................... 82
6. TROUBLE-SHOOTING THE QUICKTRACE M-6100 .............................. 86
6.1 CANNOT ZERO INSTRUMENT............................................................... 86
6.2 DRIFTING BASELINE .............................................................................. 86
6.3 LOW ABSORBANCE OR NO MERCURY RESPONSE .......................... 87
6.4 NO LIQUID OR GAS FLOW ..................................................................... 88
6.4.1 If No Sample or Rinse Flow ................................................................. 88
6.4.2 If No SnCl2 Flow ................................................................................. 88
6.4.3 If No Drain Flow.................................................................................. 88
6.4.4 No Gas Flow or Low Gas Flow ........................................................... 89
6.5 DOUBLE PEAK WITH LOW ABSORBANCE......................................... 90

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 QuickTrace Mercury Analyzer Operator’s Manual
Contents

6.6 POOR REPRODUCIBILITY.......................................................................91

6.7 NOISY BASELINE .....................................................................................92
6.8 BAD DL .......................................................................................................93
6.9 SUDDEN STANDARD ABSORBANCE RISE DURING RUN ................93
6.10 POOR ACCURACY ..................................................................................93
GLOSSARY...........................................................................................................96

QTA / M6000 SPARE PARTS ...........................................................................100

xvii
QuickTrace Mercury Analyzer Operator’s Manual
Contents

xviii
Preface
 QuickTrace M-6100 Mercury Analyzer Operator’s Manual
Preface

0. Preface
The QuickTrace M-6100 Mercury Analyzer Operator’s Manual provides
an overview and explains the theory of operation of the CETAC
QuickTrace M-6100 Mercury Analyzer. It also supplies QuickTrace
M-6100 installation and operation information, technical specification
data about the systems and sub-systems, and it details troubleshooting
and maintenance procedures.

0.1 Who Should Read This Book

The primary audience for the QuickTrace M-6100 Mercury Analyzer
Operator’s Manual consists of laboratory managers, chemists,
technicians, field-service engineers and owners of the QuickTrace
M-6100. To use this manual (and product) safely and effectively, at least
a general knowledge of chemistry, electronic or laboratory equipment,
and basic chemical handling procedures are required.

Before operating the QuickTrace M-6100, or ASX-400, it is

WARNING
important to read this manual, the QuickTrace M-6100 Mercury
Analyzer Software Manual, and the ASX-400 Autosampler
Operator’s Manual.

0.2 How to Use This Book

The QuickTrace M-6100 Mercury Analyzer Operator’s Manual contains 6
chapters. Read the chapters sequentially the first time. Thereafter,
refer to the chapters separately as needed. The first chapter provides an
introduction, system features and performance specifications for the
QuickTrace M-6100 Mercury Analyzer. Subsequent chapters detail the
installation, theory of operation, operation, maintenance, and

xx
 QuickTrace M-6100 Mercury Analyzer Operator’s Manual
Preface

troubleshooting procedures associated with the QuickTrace M-6100.

These 6 chapters are followed by a Glossary of terms.

0.3 Conventions Used in This Book

This book uses certain conventions to distinguish different types of
information. This section describes these conventions.

Instructions

All step-by-step instructions are numbered and in bold, as in the

following example.

1 Remove the Gas-Liquid Separator.

Many numbered instructions are followed by more detailed

explanations.

Menu Items

This book uses the following format for referring to menu items in the
software:

Setting|Communication

The text before the arrow symbol is the name of the menu; the text after
the arrow symbol is the menu choice.

Notes

Notes contain a reminder about the effect of particular actions. They

are indicated as follows:

xxi
 QuickTrace M-6100 Mercury Analyzer Operator’s Manual
Preface

Note:

This example shows how a note is displayed.

Cautions

Cautions indicate situations that require immediate attention to prevent

harm to the QuickTrace M-6100 Mercury Analyzer System. Cautions
are indicated as follows:

This example shows how a caution is displayed.

CAUTION

Warnings

Warnings indicate situations that could cause bodily harm. Warnings

are indicated as follows:

This example shows how a warning is displayed.

WARNING
0.4 Terminology
Terminology used in this manual may be found in the Glossary at the
end of the manual.

0.5 Where to Go for More Information

In addition to the QuickTrace M-6100 Mercury Analyzer Operator's
Manual, the analyst can refer to the following resources:

The QuickTrace M-6100 Mercury Analyzer Software Manual

The ASX-500 Model 510 Autosampler Operator’s Manual

The ADX-500 Auto Dilutor Manual (optional)

xxii
 QuickTrace M-6100 Mercury Analyzer Operator’s Manual
Preface

U.S. EPA Method 245.1; method for Hg determination in drinking water

U.S. EPA Method 245.7; Mercury in Water by Atomic Fluorescence

Spectrometry (Draft January 2001)

U.S. EPA, Office of Solid Wastes. SW846 Method 7470A; Mercury in

Liquid Waste (Cold-Vapor Technique)

U.S. EPA, Office of Solid Wastes, SW846 Method 7471A; Mercury in

Solid or Semisolid Waste (Cold-Vapor Technique)

American Society for Testing and Methods. ASTM D3223-91; Standard

Test Method for Total Mercury in Water

CETAC Technologies Customer Service and Support:

Tel: (800) 369-2822 (USA only)

Tel: (402) 733-2829

Fax: (402) 733-1932

E-mail: custserv@[Link]

0.6 List of Tables and Figures

Figure 2-1. Footprint of QuickTrace M-6100 Mercury Analyzer System...............10
Figure 3-1. Front Assembly of QuickTrace M-6100, ASX-400, and Peristaltic
Pump................................................................................................................16
Figure 3-2. Rear View of QuickTrace M-6100, ASX-400, and Peristaltic Pump...17
Figure 3-3. M-6100 Electrical Connections............................................................18
Figure 3-4. COM settings ........................................................................................23
Figure 3-5. ASCII setup...........................................................................................24
Figure 3-6. Expanded Rear View of QuickTrace M-6100......................................26
Figure 3-7. Pump Tubing Placement. ......................................................................30
Figure 3-8. Tees.......................................................................................................31
Figure 3-9. Connect the Liquid Mix, Drain, and Waste Lines .................................32
Figure 3-10. Connect the Reagent Sipper and Sample Probe ..................................33
Figure 3-11. Rinse Station and Rinse Station Pump ................................................34
Figure 3-12. Channel 1 outlet routing......................................................................35

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QuickTrace M-6100 Mercury Analyzer Operator’s Manual
Preface

Figure 3-13. Channel 2 inlet routing ....................................................................... 35

Figure 3-14. Rinse Uptake ...................................................................................... 36
Figure 3-15. Rinse Return ....................................................................................... 36
Figure 4-1. QuickTrace M-6100 Systems Functional Block Diagram ................... 43
Table 4-1 – M-6100 Carrier Pressure vs. Flow....................................................... 50
Figure 4-2. Wetting the GLS.................................................................................. 52
Table 4-2A. PPT Parameters to Optimize.............................................................. 56
Figure 4-3A. Typical Results from PPT Settings. .................................................. 56
Table 4-2B. PPB Parameters to Optimize.............................................................. 57
Figure 4-3B. Typical Results from PPB Settings. .................................................. 57
Figure 5-1. Optical Access door of QuickTrace M-6100 Mercury Analyzer......... 65
Figure 5-2. Optical cabinet of QuickTrace M-6100 Mercury Analyzer. ................ 66
Figure 5-3. Cell assembly diagram......................................................................... 68
Figure 5-4. Open end of cell end cap. .................................................................... 69
Figure 5-5. Engaged O-ring. Shown without the window and cell cap. ................ 70
Figure 5-6. Engaged O-ring. Shown with the window and the cell cap................. 70
Figure 5-7. O-ring NOT engaged. .......................................................................... 71
Figure 5-8. GLS Removal ....................................................................................... 73
Figure 5-9. Tubing Diagram and Connection Table............................................... 74
Figure 5-10. Tube routing. ..................................................................................... 75
Figure 5-11. Assembled gas-liquid separator. ........................................................ 76
Figure 5-12. Nafion®Cartridge.............................................................................. 78
Figure 5-13. M-6100 Optical Rail.......................................................................... 83

xxiv
1

Introduction
QuickTrace M-6100 Mercury Analyzer Operator’s Manual
Introduction

1. Introduction

1.1 Overview
The QuickTrace M-6100 Mercury Analyzer is specifically designed to
measure trace levels of mercury in aqueous solution by (CVAAS) Cold
Vapor Atomic Absorption Spectrometry (i.e. without use of flame,
plasma, furnace, etc.). Modular design permits remarkably easy
maintenance access and a reduced countertop footprint. Sturdy
construction, drift-stabilized double beam optics, thermal and electro-
optical lamp stabilization, and an unusually stable “non-foaming” Gas-
Liquid Separator ([Link] #5,792,663) collectively afford exceptional
structural integrity and signal stability. The QuickTrace M-6100
exhibits ultra-low signal noise and detection limits for an absorbance
system that is fully compliant with EPA method #245.1.

1.2 System Features

Principal features of the QuickTrace M-6100 Mercury Analyzer:

The QuickTrace M-6100 incorporates the following features to form an

automated, integrated Mercury analysis system.
Computer-controlled 4-channel high-performance peristaltic pump (12-
roller pump head).
• Ozone-free Hg Lamp. No lamp ventilation is needed.
• Thermally controlled Hg lamp housing (for a stabilized Hg vapor
lamp).
• Computer controlled Hg lamp power for lamp life extension.
Stable high performance Gas-Liquid Separator (GLS). (U.S. Patent
#5,792,663). Non-foaming/non-bubbling "thin liquid film" GLS
design, which allows trouble-free direct analysis of blood, urine, and
fish tissue digests as well as standard water and waste analysis.

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` QuickTrace M-6100 Mercury Analyzer Operator’s Manual
Introduction

• Rigid, shock and vibration-isolated optical rail (mounting the Hg

lamp, collimator lens, absorption tubes, camera, photo detector, and
A/D converter).
Precise, self-aligning optical mounts, no optical alignment required,
maximizing the convenience of instrument baseline zeroing. This
design extends maintenance intervals without loss of performance.
• Long path (220 mm) absorbance cells.
• Hg lamp electro-optical feedback beam utilizing a high-performance
solid-state detector for ultra-fine lamp stabilization.
• Fixed Optical Interference filters, 3 each (254 ± 2nm wavelength,
20%T, 12.7 mm dia.). No moving parts.
Standard Nafion® dryer cartridge eliminates the need for Mg(ClO4)2
drying agent.

• Stabilized double beam optics - traditional double-beam (sample and

reference) with a CCD detector.

• Internal ADC (Analog-to-Digital Conversion).

• High-rate data sampling.

Computer controlled system shutdown/standby routines.
• Integrated ASX-400 Autosampler for accommodation of calibration
standards and up to 90 samples.
• RS-232 serial communications.
• Gas exhaust Hg vapor safety trap (solid crystalline KMnO4).

1.3 System Performance Specifications

Principal performance specifications of the QuickTrace M-6100
Mercury Analyzer:

• Low detection limits: typically < 10ppt at 20mL / min. carrier gas
flow **. (Direct steady state absorbance mode, without
preconcentration by gold amalgamation).
• Wide dynamic linear working range, ≅ 6 orders of magnitude.

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QuickTrace M-6100 Mercury Analyzer Operator’s Manual
Introduction

• Short term precision, maximum 1.5% RSD, typical ≤ 1% RSD**.

• Ultra-low drift rates ≤ 300µAbs/hr (after warm-up) raw uncorrected
analog baseline on-screen drifts.
• Ultra-low short-term absorbance noise ≤ 100 µAbs (10-5 Abs).
• 0.1% "raw" Hg lamp stability (single beam output).
• Unusually fast washout ≈ 180 sec. from 1ppm Hg, at 350mL/min gas
flow.
• Mercury Response: ≥ 6000 µAbs / ppb* at 100mL/min carrier gas
flow.

* Using prescribed tubing, reagents, and pump speed.

** 1 hour minimum warm-up using the standard Nafion® dryer and a

gas flow equal to 20mL/min along with prescribed tubing and reagents.
Using pump speed, uptake and rinse times specified for standard
Nafion® Dryer in Table 1-1, and <16 s integration cycle selected on the
"flattest" portion of the peak time profile.

4
2

Preparing for Installation

QuickTrace M-6100 Mercury Analyzer Operator’s Manual
Preparing for Installation

2. Preparing for Installation

Installing the QuickTrace M-6100 requires preparation. This chapter
discusses what requirements must be met when obtaining supplies and
choosing a location for the QuickTrace M-6100. It also describes how to
successfully unpack the system prior to installation. Before installing
the Mercury Analyzer, first obtain the necessary supplies listed below.
Next evaluate the laboratory layout to choose a suitable location. Once a
location is chosen, carefully unpack the QuickTrace M-6100 prior to
installation.

If a computer was purchased from a source other than CETAC, see the
QuickTrace Mercury Analyzer Software Manual for details on how to
install the QuickTrace software.

2.1 Supplies

2.1.1 Necessary Supplies

• Inert Gas Regulator.

2-stage, 10-200 psig secondary pressure gauge, with plumbing

couple for either a cylinder or dewar capable of delivering 150 psig.

• AC Power Strip (surge protected) with 6 outlets.

• Cylinder or Dewar, UHP Nitrogen or Ar gas.

Ultra-high purity, dry, research grade N2 or 99.999% purity Ar. The

QuickTrace M-6100 has a user replaceable 2-micron filter, which
prevents damage from particulates to the internal gas control
components.

• Mercury Standard Solution.

1000 ppm (minimum order quantity).

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 QuickTrace M-6100 Mercury Analyzer Operator’s Manual
Preparing for Installation

• Hydrochloric Acid Trace Metal Grade (37%).

Trace metal HCl will be used in the preparation of Hg standards,

SnCl2 reagent and in some method applications. If an application is
more demanding, a better grade of acid may be needed (e.g. double
distilled).

• Nitric Acid Trace Metal Grade (68-70%).

Trace metal HNO3 will be used in sample preparation, cleaning

glassware (lab glassware and the QuickTrace gas liquid separator)
and added to the QuickTrace rinse solution to help maintain the
cleanliness of the system during operation.

• Stannous Chloride (Crystals, Di-Hydrate).

2-500g containers minimum order, “suitable for Hg determination.”

The stock SnCl2 is introduced into the QuickTrace at a steady flow
rate and therefore any Mercury contamination will be negated
during the instrument zero.

• Potassium Permanganate. Solid, crystalline.

The cheapest available grade at a minimum quantity is sufficient

unless it is also to be used for oxidative sample preparation. This low
grade reagent stock is sufficient to fill a safety trap for retention of
Hg vapor exhaust from the instrument.

• 2-Propanol. High purity, “spectrophotometric” grade.

2-propanol will be used for cleaning the optical cells and cell
windows.

• Kimwipes.

• Additional Chemical Compounds.

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The sample preparation procedures of the intended analytical

method may require additional chemical compounds. Refer to
published method specifications.

2.1.2 Recommended Supplies

• Volumetric Flasks 100mL class A (TC) 6 each.

• Volumetric Flasks 1000mL class A (TC) 2 each.

• Precision Automatic Micropipettes, 10 to 1000 µL (TD).

• Replacement Tips for Micropipettes.

• Disposable Plastic dropping pipettes.

• Graduated Cylinders, 10 and 100 mL.

• Polypropylene or Polyethylene Bottle with Cap, 1 L.

• Weighing Balance, Top Loading, 0.1g readability (or better), any

available capacity will work (1.1 Kg capacity is good).

• Laboratory Scoopula and Large Spatula.

• Stop-Watch (for measuring liquid uptake rates).

• Stirring Rod.

• Powder Funnel, wide bore stem, small overall size.

• Wrenches, adjustable 12” and 6”.

• Screw Drivers:
1 small Phillips
1 medium Phillips
1 long-shank medium flat-blade

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Preparing for Installation

1 small thin flat-blade

• Deionized Water.

• Flow Meter 0 - 500 mL/min. with 1 mL/min. readability, calibrated

to user’s choice of carrier gas (Ar or N2).

2.2 Choosing a Location

Choosing a location for the QuickTrace M-6100 involves evaluating the
laboratory environment for the availability of space, ventilation and
power. For the QuickTrace M-6100 to function optimally, the location
selected must meet specific requirements associated with each of these
items. The following sections discuss space, ventilation and power
requirements.

2.3 Space Requirements

The QuickTrace M-6100 Mercury Analyzer System which includes the
base unit, Autosampler and peristaltic pump requires a minimum
footprint for countertop installation of 70 cm x 70 cm x 76 cm (WxDxH).
A floor space of 30 cm x 30 cm is required for the liquid waste receptacle.
The space for the waste can be directly below the analyzer, or directly in
front of the lab bench and inline with the peristaltic pump. The
computer used to operate the QuickTrace Mercury system needs a
minimum space of 60 cm x 70 cm x 60 cm (WxDxH). At a very minimum,
the overall width required is 150 cm to accommodate the QuickTrace
and computer. See figure 2-1.

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Preparing for Installation

FRONT SIDE

ASX-400
ASX-400

REAGENT PERI PUMP

BOTTLE
M-6100
Allow
10cm RINSE
M-6100 for BOTTLE
cords

73cm 53cm

Figure 2-1. Footprint of QuickTrace M-6100 Mercury Analyzer System.

2.4 Ventilation
During operation, the QuickTrace M-6100 internally contains trace
amounts of mercury vapor. To prevent inhalation of the vapor, the
QuickTrace M-6100 uses a solid KMnO4 absorbent trap located on the
back of the instrument. This trap absorbs the mercury vapor prior to
final exhaust; therefore no extra ventilation is required beyond that of a
standard laboratory environment.

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Gases exhausting from the QuickTrace M-6100 cabinet, prior to

WARNING
the external Hg vapor trap (affixed to the rear cabinet panel)
contain traces of mercury vapor and must be treated as such. Do
not run the QuickTrace M-6100 unless exhausted gas is properly
“scrubbed” or removed. Either fill, maintain, and use the
provided KMnO4 absorbent trap or run a transfer line to a fume
hood.

Locating the QuickTrace M-6100 directly in the path of an air

conditioner or heater vent may cause baseline drift, and is not
recommended.

Notice:

Due to the likelihood of accelerated damage from corrosion and dust,

operating the QuickTrace M-6100 in a fume hood with stagnant air
automatically voids the warranty.

2.5 Power Requirements

Place the QuickTrace M-6100 within 1.2m of a standard power outlet.
The QuickTrace M-6100 instrument and peristaltic pump power input
requirements are specified when ordering, either 115 VAC (50/60 Hz) or
220-240 VAC (50/60 Hz). Five power outlets are required, for the
QuickTrace M-6100 Mercury Analyzer, Peristaltic Pump, ASX-400
Autosampler, computer, and monitor. (An AC surge protected power
strip with 6 or more outlets will suffice).

The QuickTrace M-6100 base unit, Autosampler, and peristaltic pump

have “universal voltage” input. They use an external switching power
supply to supply power at +24 VDC to the system.

The power cord set supplied with the QuickTrace M-6100, ASX-400, and
Peristaltic pump meets the requirements of the country where the
instrument was purchased. If the instrument is to be used in a country

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Preparing for Installation

other than the one specified at the time of ordering, obtain a new power
cord set that meets the requirements of that country.

This equipment is designed for connection to a grounded

WARNING
(earthed) outlet. The grounding type plug is an important safety
feature. For continued protection against electrical shock or
damage to the instrument, do not disable this feature.

2.6 Unpacking the QuickTrace M-6100

Inspect the external packaging upon receipt for holes, tears, smashed
corners, water damage or any other outward signs of damage from
rough handling or abuse during shipment. Notify the shipping
carrier of the damage to the shipping container and open
immediately to inspect for damage. Inspect all items during
unpacking and notify the carrier immediately of any concealed damage.

If the QuickTrace M-6100 or any of its components are shipped or

removed from storage during cold weather, allow the packaged
equipment to attain room temperature before opening and exposing to
warm, humid air. It is usually sufficient to provide 4 to 8 hours for this
purpose.

If water damage has occurred (en route or at destination), or if

condensation forms on or inside the QuickTrace M-6100 system, allow it
to dry thoroughly before connecting it to an AC power source and
operating it. Failure to do so may cause equipment damage. Also, notify
CETAC Customer Service if any damage is revealed upon inspection.

Remove the packing checklist from the shipping container, and check off
items against it. Leave accessories in the packing until needed.

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Note:

Do not throw away the factory packaging. Keep it for possible future use.

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14
3

Installing the
QuickTrace M-6100
 QuickTrace M-6100 Mercury Analyzer Operator's Manual
Installing the QuickTrace M-6100

3. Installing the QuickTrace M-6100

Refer to figures 3-1 and 3-2 to identify specific components on the

analyzer.

Z-Axis Drive
ASX-400 Autosampler

Sample Probe Holder

Sample Probe

Standards Rack

Rinse Station
Auto-sampler Tray

M-6100 Base Unit

Rinse

Front Door

Tubing Bridge

Peristaltic Pump
Reagent

Figure 3-1. Front Assembly of QuickTrace M-6100, ASX-400, and Peristaltic Pump.

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Installing the QuickTrace M-6100

Sample Probe Holder

ASX-400
Auto-sampler Sample Probe

M-6100 Base Unit

Power In
Z Drive

Rinse Station Pump Peristaltic Pump

Lamp Power
Tubing Bridge
Power In

Mercury Trap Holder

Gas Inlet/Exhaust
Power In Reagent

Rinse

Figure 3-2. Rear View of QuickTrace M-6100, ASX-400, and Peristaltic Pump.

3.1 Placement of the ASX-400 Autosampler

and Peristaltic Pump
1. Place the ASX-400 autos-ampler on top of the QuickTrace
M-6100 base unit.

The placement is such that the autosampler tray is touching the front
cabinet of the base unit.
2. Place the analytical Peristaltic Pump directly to the left of the
QuickTrace M-6100 base unit.

Leave an ~1cm gap. The pump should also be set back so that its front
edge is approximately in line with the boundary between the
QuickTrace M-6100 base unit and the front cabinet.

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3.2 Electrical Connections

Refer to figure 3-3.

Blue
(COM1)

24 VDC Power
(jack connector)

Purple-Yellow-Green (PYG)
(Auxillary and Peripheral Interface)

24 VDC Power
(6-pin connector)

Orange
(Computer Interface)

24 VDC Power
(6-pin connector)

Figure 3-3. M-6100 Electrical Connections

Three power cords and universal 24 VDC power adapters are

included with the QuickTrace M-6100 system.
1. Place the on/off switches on the power adapters in the off
position.
2. Check that the base unit’s lamp power switch immediately
below item is off (released “out” rather than pushed “in”).
3. Check that the main power switch to the ASX-400 is off
(released “out” rather than pushed “in”).
4. Check that the main power switch to the peristaltic pump is
in the off position.

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Installing the QuickTrace M-6100

5. Insert the male jack plug from the power adapter into the
female 24 VDC-in jack on the ASX-400.
6. Insert the male six-pin plugs from the power adapters into
the female 24 VDC-in connectors on the M-6100 base unit and
Peristaltic Pump.
7. Connect the power cords to the 24 VDC power adapters, then
insert the other ends into a grounded surge protected power
strip.
8. Plug the surge protection power strip into the AC outlet
receptacle.
Do not apply power to the QuickTrace M-6100 at this time.

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3.3 PC Interface
Refer again to figure 3-3.

The system utilizes a nine pin male RS232 serial communication port
(BLUE) for the ASX-400 autosampler, and a high-density 50-pin
connector (ORANGE) for the QuickTrace M-6100 Mercury Analyzer base
unit. These can be found the completion kits.
1. Connect the blue labeled cable to the ASX-400 blue (COM1)
port.
2. Connect the other end of the blue labeled cable to the
computer COM1.
3. Connect the orange labeled cable to the M-6100 orange
(COMPUTER) port.
4. Connect the other end of the orange labeled cable to the
computer orange (acquisition card) port.

3.4 Autosampler and Peristaltic Pump

Auxiliary Cables
Refer again to figure 3-3.

Locate the purple-yellow-green (PYG) auxiliary cable in the QuickTrace

M-6100 completion kit.
1. Connect the green end of the PYG cable to the ASX-400 green
(AUXILLIARY) port.
2. Connect the yellow end of the PYG cable to the M-6100
yellow (AUXILLIARY) port.
3. Connect the purple end of the PYG cable to the Peristaltic
Pump purple (CONTROL) port.

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Installing the QuickTrace M-6100

3.5 Installing the Autosampler Z Drive

and Sample Probe
See the ASX-400 Autosampler Operators Manual, and follow the
instructions carefully.

3.6 Verifying the Installation

Once installation of the QuickTrace M-6100 system is complete, it is
important to verify that the system is installed correctly.

CAUTION Attempting to use the QuickTrace M-6100 before ensuring that all
components are installed correctly may result in damage to the system.

3.6.1 Testing the Interface

0. Install the QuickTrace M-6100 software at this time if a PC
was purchased from a source other than CETAC. It is
important to view and understand the [Link] file
following the installation of the software.
1. Power on the QuickTrace M-6100, ASX-400, and Peristaltic
pump. (In addition to the power switches on the
instrumentation, there are switches on the 24V power
supplies)
2. Power on the M-6100 Lamp.
3. Check to ensure that the auxiliary port cables are connected
to the equipment according to sections 3.3 and 3.4.
4. Start the QuickTrace software.
5. When the software is initializing, it will test the connections
to the Peristaltic Pump, QuickTrace M-6100 Instrument (base
unit) and the ASX-400 Autosampler.

The QuickTrace M-6100 software runs a test routine at startup to test

the various interfaces throughout the system. The software will give a
report on the status of the interface if there is a failure.

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Installing the QuickTrace M-6100

3.7 Verify the Software Configuration of COM

Ports Manually
If the software does not find the QuickTrace M-6100 base unit or
the ASX-400 autosampler it will be necessary for the analyst to
test them using the QuickTrace software and the
[Link] program provided with Windows

To check or change the configuration in the QuickTrace software:

1. Open the Specify Installed Hardware application, in the

Start menu.

2. Verify that the Autosampler is connected to the correct COM

port. The default configuration is ASX-400 Autosampler on
COM1. If the configuration differs from the default, set the
Autosampler to COM1.

3. Press okay to save changes and exit the application.

4. Restart the QuickTrace software.

If errors persist, the Windows’ HyperTerminal program can be used to

manually verify the communication through each serial port.

3.7.1 Using Windows HyperTerminal Program

HyperTerminal (if installed) can be found in the Start menu. Select the
Programs | Accessories | Communications folder to find the HyperTerminal
program.

Note:

This manual assumes the reader and operator of the QuickTrace

M-6100 Mercury Analyzer has a working knowledge of using standard
Windows applications. For more information on how to use Windows,
see your computer’s documentation.

1 Click on [Link]. (It may be designated HyperTerminal.)

2 If this is the first time that HyperTerminal has been run on
this computer, you may be asked to enter an area code and

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Installing the QuickTrace M-6100

other dialing information. This information will not be used

for our procedure, so enter any number you desire.
Furthermore you may be prompted to install a modem – this is
not necessary and can be ignored.
3 A dialog box titled "Connection Description" will appear. Enter
a name significant to you, such as "QuickTrace M-6100 ".
4 A dialog titled "Phone number" or "Connect to" will appear.
The only important field is the "connect using" field. Select
"Direct to com1" or "COM1".
5 A COM port properties dialog box will appear. Be sure the
settings are as follows: 9600-8-N-1 (9600 baud, 8 data bits, no
parity, 1 stop bit) with no flow control. (As illustrated in the
figure 3-4)

Figure 3-4. COM settings

6 Under the file menu select “Properties”.

7 A properties dialog box will appear.
8 Click on the setting tab. Click on the “ASCII Setup…” button.
A dialog box will appear. Make sure the following settings are
checked (figure 3-5).
“Echo typed characters locally”
“Append line feeds to incoming line ends”

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Installing the QuickTrace M-6100

Figure 3-5. ASCII setup

9 Click OK to confirm these settings.

10 Go to file menu and select Save.

If you have changed the COM port properties, you may have to sever
your connection and reconnect to have the new settings take effect. This
can be done using two buttons on the toolbar – the one with the phone
off the hook disconnects, the one with the phone on the hook reconnects.

The ASX-400 will respond to the command VER (capitalization is

important).

The Autosampler will respond ‘CETAC Technologies ASROM...’. If the

response is not received as expected on the expected COM ports, then
this will indicate a hardware or Windows configuration problem.

3.8 Checking the Autosampler Components

See the ASX-400 Autosampler Operator’s Manual to verify
configuration.

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Installing the QuickTrace M-6100

3.9 Testing the Sample Probe

Refer to the ASX-400 Autosampler Operator’s Manual and the
QuickTrace Software Manual to verify proper alignment and movement
of the ASX-400.

3.10 Carrier Gas Connection

Refer to Figure 3-6. Locate the plastic-shipping bag labeled "Completion
Kit - QuickTrace M-6100 ". It contains various small parts, tubing,
fittings, computer CD-ROM, etc. In this bag, find the brass 2-micron gas
filter, with associated brass Swagelok™ fittings, and a short section of
ETFE tubing (attached to the filter) which has been formed into a
partial loop.

Install the looped end of the ETFE tube into the bulkhead fitting labeled
“GAS INLET", and tighten the fitting very securely. Make sure that the
flow arrow on the gas filter is pointing in the direction to the gas in
fitting.

Determine how far the QuickTrace M-6100 is located from the gas
supply (UHP nitrogen or argon). Allowing a generous service loop cut an
appropriate length of 1/8" nylon tubing from the roll provided. Connect
one end of this tube to the gas inlet side of the 2-micron brass filter and
tighten the Swagelok™ fitting securely.

Note:

A 2-micron in-line filter must always be used. The 2-micron filter has been
selected for minimal pressure drop and minimal flow fluctuation. Do not
substitute other filters.

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Installing the QuickTrace M-6100

Mercury vapor trap

2 micron gas filter

Figure 3-6. Expanded Rear View of QuickTrace M-6100.

Connect the other end of the nylon tube to the gas supply regulator, using ¼”
NPT 1/8” Swagelok™ fitting provided.

Note:

Exceeding 120 psig gas supply pressure to the QuickTrace M-6100 may
rupture the bulkhead fittings, causing the unit to malfunction.

Use only “research-grade”, “dry” UHP nitrogen or argon. Do not use “welding”
CAUTION
grade gases - these may permanently damage the QuickTrace M-6100.

3.11 Mercury Trap (KMnO4)

In the plastic bag labeled "Completion Kit - QuickTrace M-6100 ", find the
polyethylene tube with a 7 inch (17.8 cm) length of dark Viton tubing
attached to one end. When filled with crystalline potassium permanganate,
this will serve as the mercury vapor trap. The vapor trap will clean the

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Installing the QuickTrace M-6100

QuickTrace M-6100 exhaust vapors, to prevent the release of mercury vapor

into the lab atmosphere.

Refer back to Figure 3-6. Remove one end cap from the polyethylene tubular
body. Do NOT remove the heatshrink wrapped Luer fitting from the end cap.
Inspect both end cap interiors to ensure that the ends are lightly plugged
with fine glass wool. If not, lightly pack a small loose wad of fine glass wool
into the small i.d. section of each cap. Pack enough glass wool to stop the
potassium permanganate from filtering through, but not restrict the gas flow.
Once the glass wool is in place, use a powder funnel to fill this tube with dry
crystalline solid potassium permanganate (KMnO4). While filling, have one
end fully capped, hold the other end straight upward, and use the powder
funnel to guide the KMnO4 crystals into the tube. Fill to the top, tapping a
finger lightly on the tube to settle the KMnO4, and finally place the end cap
on securely.

Be sure to wear protective eyewear and safety gloves when

WARNING
handling chemicals.

Refer again to Figure 3-6. Snap the filled mercury trap into the black
holders under the silk-screen label "MERCURY TRAP (KMnO4)". Attach
the black Viton tube to the PTFE tubing labeled "GAS EXHAUST". The
Mercury vapor trap needs to be cleaned and refilled when the brown
color approaches the open end. This is the formation the MnO2 as the
KMnO4 is reduced. The Potassium permanganate may last at least one
year depending on frequency of use, except in the unlikely event of a
major overflow accident in the QuickTrace M-6100.

Note:

So long as the KMnO4 is dry, free flowing (not caked), dark purple
crystals, it is perfectly OK.

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3.12 Nafion® Dryer Cartridge

CETAC’s Nafion®-based dryer cartridge1 (figure 4-3 (L)) is designed as
the standard recommended drying system for all CETAC Mercury
Analyzers (it replaces the older magnesium perchlorate drying tube).
Using the Nafion® dryer substantially reduces daily maintenance and
setup time, since daily water saturation will not occur with the Nafion®
membrane as it may with the earlier magnesium perchlorate system. It
also lowers detection limits and yields more consistent performance.
Nafion® cartridges typically last 3 to 6 months whereas older
magnesium perchlorate systems must be replaced/recharged at least
once a week (if not daily).

Nafion® Dryer benefits:

• Efficient drying capability.

• No maintenance required.

• Improved long-term precision.

• Higher sensitivity.

• Lower detection limits.

• User can easily interchange Nafion® and perchlorate cartridges, if

desired (but the Nafion® cartridge is recommended for all
applications).

• Replace Nafion® cartridge every 3 to 6 months, depending on use.

The CETAC Nafion® dryer cartridge contains a tubular inner Nafion®

membrane housed within an outer tube and coiled inside the cartridge.
The argon or nitrogen carrier gas containing mercury and water vapor is
swept along the inner Nafion® membrane, allowing water vapor to
permeate the membrane selectively, whereas the membrane is not
permeable to mercury vapor. On the “waste” side of the membrane, a
counter gas flow, split from the carrier gas supply, selectively sweeps
the water vapor out of the system, whereas non-permeating mercury
vapor proceeds to the sample cell.

1
Nafion® is a registered trademark of DuPont (E.I. du Pont de Nemours and
Company), which trademark is licensed to Perma Pure, Inc. and used (with
permission) herein by SD Acquisition, Inc. DBA CETAC Technologies.

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The CETAC Nafion® dryer cartridge and associated plumbing is already

pre-installed in your new QuickTrace M-6100 factory shipment. No
further installation is required.

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3.13 Plumbing Connections

Refer to figures 3-7 to 3-10.

3.13.1 Installing the Peristaltic Pump Tubing

1 Release all four peristaltic pump channel clamps.

2 Locate the peristaltic pump tubing in the completion kit. There

are two sets of pump tubing. The tubes with the yellow bridge
stops are for the sample and drain channels. The tubes with
the black bridge stops are for the reagent channel.

3 Install tubes with yellow bridge stops in the first three

channels.

4 Install a tube with black bridge stops in the top channel.

4
3 Liquid Mix
Black
2
1
Channels

Yellow

Drain

Dryer Exhaust

Figure 3-7. Pump Tubing Placement.

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Installing the QuickTrace M-6100

3.13.2 Installing the Mixing Tee and Drain Tees

1 Locate the smallest (1/16” dia.) polypropylene provided in the

completion kit. Install this tee on the destination side of the
pump. It connects the top two channels.

2 Connect the remaining two larger (3/32” dia.) tees to the two
peristaltic pump drain tubes.

Small (1/16”) Tee

“Large” (3/32”) Tees

Figure 3-8. Tees

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3.13.3 Connecting the Liquid Mix and Drain Lines

1 Connect the Liquid Mix line to the small tee on the outlet side
of channels 3 and 4.

2 Connect the Drain line to the ‘large’ tee on the inlet side of
channels 1 and 2.

3 Locate the 3 foot long waste line (1/8” o.d. Tygon tubing) in the
completion kit, and connect it to the ‘large’ tee on the outlet
side of channels 1 and 2.

4 Find a Luer male barbed fitting (look for this in the 10 liter
waste container). Replace one of the luer caps on the waste
container lid with the barbed fitting. Attach the other end of
the waste line to this fitting.
To prevent pressure buildup in the 10l waste container, be sure that at
least one of the two vents on the 10l waste container are open
(uncapped) during operation.

Liquid Mix

Waste
Drain

To Waste
Container
Figure 3-9. Connect the Liquid Mix, Drain, and Waste Lines

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3.13.4 Connecting the Reagent sipper tube and

Sample Probe

1 Find the 11 inch (28cm) length of 1/16” Teflon tubing inside the
Reagent Bottle. This is the “Reagent Sipper Tube”.

2 Fill and cap the Reagent Bottle with 10% SnCl2 (in 7% HCl v/v).
The reducing agent will be used with the QuickTrace M-6100
system during operation of the system. Cap the Luer fitting
when not in use to preserve the SnCl2.

3 Connect the 11 inch Reagent Sipper Tube to the inlet side of

channel number 4.

When in use, to ensure that no precipitated solids are pumped through the
system, the reagent tube should not touch the bottom of the Reagent Bottle.

4 Connect the 1/16” Teflon tubing from the sample probe to the
inlet side of channel number 3.

To
Sample
Probe
Reagent
Sipper
Tube

Reagent
Figure 3-10. Connect the Reagent Sipper and Sample Probe

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3.13.5 Connect the ASX-400 Rinse Station Tubing

The ASX-400 autosampler peristaltic rinse pump rotates clockwise. The

rinse station is always filled from the Fill (bottom) port and drained
from the Drain (top) port. For a full description of how to set up the
ASX-400 rinse station tubing, see the ASX-400 Autosampler Operator’s
Manual.

Rinse Station

Channel 2 outlet Drain

Rinse Channel 1 outlet
Station
Pump

Channel 1 inlet
Channel 2 inlet Fill

Rinse Bottle

Figure 3-11. Rinse Station and Rinse Station Pump

Fill the rinse bottle with trace metal grade 1% HCl/HNO3 v/v.

Note:

When analyzing samples and standards of high concentration such as

20ppb or greater use a stronger concentration of acid i.e., 5% HCl/HNO3 or
greater.

Locate in the completion kit the ¼” OD Tygon tubing and refer to

Figures 3-11 to 3-15. The tubing will need to be cut to the appropriate
lengths.

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1. Connect Channel 1 outlet to the Fill port on the Rinse Station.

Channel 1 outlet

Rinse station fill

Figure 3-12. Channel 1 outlet routing

2. Connect Channel 2 inlet to the Drain port of the Rinse

Station.

Rinse station drain

Channel 2 inlet

Figure 3-13. Channel 2 inlet routing

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3. Cut a length of tube to extend from Channel 1 inlet to the

bottom of the Rinse bottle. Connect it.

Channel 1 inlet

Rinse uptake

(to bottom of bottle)

Figure 3-14. Rinse Uptake

4. Cut a length of tube to extend from Channel 2 outlet to

dangle a few inches inside the Rinse bottle. Connect it.

Channel 2 outlet

Rinse return

(extends a few
inches into bottle)

Figure 3-15. Rinse Return

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3.13.6 Peristaltic Pump Tubing Clamp Tension

1 Disconnect the tube labeled “11Æ ÆHG VAPORÆ

Æ12” from the
GLS vapor outlet (refer to figure 4-2).

2 Open the QuickTrace software.

3 Open the QuickTrace hardware Controls (see QuickTrace

Software Manual) by pressing the Instrument button, or select
Window|Instrument.

4 With zero clamp tension on the tubing (screws nearly

unscrewed), snap all four clamps into place and start the
Peristaltic Pump.
4a Set gas pressure to 30 psi.

Read through steps 5-8 before proceeding. It is extremely

important to set the peristaltic pump drain clamps in a timely
fashion after the GLS begins to fill with liquid. Failing to do so
can cause an overflow and spillage.

WARNING Do not start liquid flow without the carrier gas being on and
pressure set to 30 psi. Otherwise, fluid backfill into the gas
ballast can occur.

Refer to software manual for instrument control.

5 Place the ASX-400 sipper tube into rinse station. Use the mouse
and click the “Up” button, then the “Park” button. Visually
verify the sipper’s movement.

6 Manually increase the clamp tension on Channel 3 until liquid

uptake begins in the sipper tube.

7 Watch the liquid flow as it makes its way from the ASX-400
rinse station, to the pump, through the mixing tee, and to the
Gas-Liquid Separator.
The GLS will begin to fill with rinse solution.

8 Increase the clamp tension on both of the drain tubing clamps

(Channels 1 & 2) until flow begins from the drain port of the
GLS and the liquid level begins to drop.

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Do this quickly before the GLS fills to the point where fluid overflows
the GLS. The GLS should slowly drain to empty, even though sample
continues to be delivered to the top of the frosted center post. The GLS is
intended to operate “empty” with only a thin film of liquid continuously
wetting the frosted center post and exiting the drain.

9 Tighten both drain tube clamps equally to ensure even flow to

each.
Check this by observing the segmented flow at both drain tees. The rate
of flow in and out should be balanced through both Santoprene drain
lines. Adjust the clamp tension to keep the GLS empty and to achieve a
smooth, balanced, segmented flow. Unstable drain flow can cause
baseline noise in the system.

10 Start the SnCl2 flow.

a Place the SnCl2 uptake tube in the reagent bottle
b Close the Channel 4 clamp.
c Increase the reagent clamp tension until reagent uptake begins in
the tube.
d Adjust the clamp so that the flow from the SnCl2 bottle is smooth,
with no jerks in the flow.

11 Once liquid is running through the QuickTrace M-6100, note

that the drain tubing clamp tension is properly adjusted by
watching the flow through the Gas-Liquid Separator.
The GLS should remain empty and liquid exiting the GLS should appear
nearly motionless, with no flutter or instability.

12 The flow into the GLS should be as smooth and pulse free as
possible.
View this closely at the top of the GLS frosted center post. The liquid
should stream continuously from the capillary tip to the top of the post,
and the liquid column spanning the gap between the capillary tip and
post should be nearly “motionless”, with minimal fluctuation and no
jerkiness or discontinuity. If this is not the case check that the “gap”
between the bottom of the GLS capillary insert tube and the top of the
GLS frosted center post is ~0.5 mm (range of 0.3-0.6 mm). If not, very
carefully slide this insert up or down, as needed. Refine the clamp
tension of the sample and reagent channels as needed to stabilize the
liquid flow to the GLS.

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A flow check with a 10ml graduated cylinder (less than 100mm tall) and
stopwatch should yield a sample uptake rate of ~5 mL/min, and a
reagent uptake rate of ~1.8 mL/min. Check liquid flow stability at the
drain exit of the GLS after final adjustments of clamp tension to sample
and reagent pump tubing.
Flow Check Procedure - Reagent
1 Fill the 10ml graduated cylinder with 10ml DI water
2 Simultaneously place the reagent sipper tube in the
graduated cylinder and start the stop watch.
3 After 30 seconds, remove the uptake tube from the cylinder.
4 Measure the water remaining in the cylinder, and calculate
the reagent flow rate.

Flow Check Procedure - Sample Probe

1 Fill the 10ml graduated cylinder with 10ml DI water.
2 Move the Sample probe to the middle of the sample rack.
(1:35 if set for a 60 position rack).
3 Position the graduated cylinder beneath the Sample Probe.
4 Simultaneously click the Down button and start the stop
watch.
5 After 30 seconds press the Up button.
6 Measure the water remaining in the cylinder, and calculate
the flow rate.
7 Park the Sample Probe.

Note:

When properly adjusted the tension on the bottom three peristaltic pump
tubes should be the same and the tension screw for the top pump tube
(reagent tube) should be screwed 1 to 2 mm farther in.

Once the clamp tension on the pump tubing is established, relieve their
stretch.
1. Unclamp reagent and sample clamps.
2. Park the Sample Probe.

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3. Press the Up button to remove the Sample Probe from the

Rinse Station.
4. Remove the sipper tube from the SnCl2.
5. Allow the waste line to empty.
6. Unclamp waste line clamps.
7. Turn the pump off using the software controls.

Do not leave tubes clamped in place when the system is not being used.
The next time the system is used, hook the tubes and close the quick-
release mechanisms. No screw adjustments will be needed. Previous
clamp tension is “remembered” as the quick release is engaged and
disengaged.

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4

Using the QuickTrace

M-6100
QuickTrace M-6100 Mercury Analyzer Operator’s Manual
Using the QuickTrace M-6100

4. Using the QuickTrace M-6100

Operation of the M-6100 is mostly through the QuickTrace Software
interface.

For a detailed description of the software see the QuickTrace Mercury

Analyzer Software Manual.

The following chapter covers physical operation instructions to achieve

optimum performance.

4.1 Theory of Operation

4.1.1 ASX-400 Autosampler

The Autosampler is prepared for operation by loading sample vials (up to

90) of digested samples, into selected positions of the sample racks. Vials of
calibration standards (up to 10) are placed in user-selected positions of the
standards rack. Rinse solution, for sample-to-sample probe
decontamination, fills the rinse station and re-circulates to the rinse bottle.

The Autosampler operates under computer control to move the sample

uptake probe to any sample position; the rinse station, reference standard,
blank, etc., in a user-programmed sequence. The sample uptake probe
(sipper tube) supplies the multi-channel peristaltic pump's sample inlet.

For further information, see the ASX-400 Autosampler Operator's Manual.

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Figure 4-1. QuickTrace M-6100 Systems Functional Block Diagram

4.1.2 QuickTrace M-6100 Automated Mercury Analyzer

[Link] Sample Introduction & Stannous Chloride Reactor

Refer to Figure 4-1 to trace the path of liquids through the M-6100 System.
An acidified digested aqueous sample from the autosampler is introduced,
via peristaltic pump as Hg2+ dissolved in solution. A reducing agent (10%
stannous chloride in 7% HCl), is introduced via a parallel pump channel.
The sample and reagent (SnCl2) streams join at the mixing tee (1), and
immediately enter the QuickTrace M-6100 tubing reactor (“Liquid Mix”).
Sn2+ reduces Hg2+ in solution to Hg0 while the mixture is en route to the
Gas - liquid separator (GLS). At this stage and prior to the GLS, the
analyte is present as a finely dispersed emulsion of liquid (metallic) Hg0
micro-droplets, in excess SnCl2 solution.

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NOTE:

The CETAC QuickTrace M-6100 Mercury Analyzer measures inorganic mercury

(free Hg2+ or HgCl2, which is subject to efficient stannous chloride reduction in the
QuickTrace M-6100 tubing reactor); using inorganic mercury standard solutions for
instrument calibration. If insoluble mercury, bound mercury, or organomercurials
are present in samples, an appropriate sample dissolution/digestion procedure will
have to be employed to convert these other forms to free inorganic Hg2+ or HgCl2,
prior to analysis with the QuickTrace M-6100.

[Link] Gas - liquid Separation

The finely dispersed Hg0/SnCl2 emulsion is introduced into the top of the
GLS (Gas - liquid Separator (2)). The Hg0/SnCl2 emulsion flows over the
frosted GLS center post in a relatively thin film, covering the entire post
from top to bottom. A carrier gas simultaneously enters the bottom of the
GLS tangentially (10). The carrier gas (Ar or N2) swirls around the wetted
center post and upwards toward the GLS gas exhaust port (11).

Hg0 droplets in the thin emulsion film quickly evaporate into the gas vortex
surrounding the post. The carrier gas stream efficiently sweeps this Hg0
vapor (along with some evaporated water) upward and out of the GLS gas
exhaust (11), and on to the drying (12, 13) and optical section (14, 15) of the
QuickTrace M-6100 for CVAAS analysis.

The liquid water, containing excess reducing agent, acid, any non-
participating "spectator ions", and reaction by-products, finally drains out
the bottom of the GLS (3) and is pumped to waste (4) (channels 1 & 2).

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Note:

The GLS operates “empty” with no liquid level. The liquid spreads out
as a film that wets the center post. At the bottom of the post, the film
collects at a single point and is then continuously pumped to waste, so
the “liquid level” should not rise in the GLS.

[Link] Carrier Gas

Refer again to Figure 4-1 to trace the path of the carrier gas. A clean, dry
carrier gas, such as UHP N2 or Argon, must be supplied to the back of the
instrument. The gas passes through fixed restrictors to produce primary
flow rates in the range of 20-350 mL/min @ 10-100 psig. The carrier gas
first enters the reference cell (6) to facilitate measurement of the incident
radiant power (P0) at 253.7nm. It exits (7) and passes through the GLS (10)
to pick up Hg0 vapor from the reduced sample. The carrier gas and Hg0
vapor exit the GLS (11) and enter (12) a Nafion® drying cartridge where
water vapor is removed (13). For the Nafion® dryer, an auxiliary sweep gas
from a restrictor (5A) enters an auxiliary port (12A) and selectively removes
water vapor from the dryer cartridge at 13A.

Finally, the dry Hg0/carrier gas mixture exits the dryer (13) and enters the
sample cell (14) for measurement of transmitted radiant power (P) at 253.7
nm.

Ultimately, the gas stream (carrier gas and Hg0) exits the sample cell (15)
and is exhausted to a solid KMnO4 trap (16) where Hg0 is absorbed, and
clean carrier gas passes to the lab atmosphere.

[Link] Optics and Cold Vapor AAS

Refer again to Figure 4-1 to trace the optical path of the QuickTrace
M-6100. The Cold Vapor AAS (Atomic Absorption Spectrometry) process
within the sample cell begins with a low pressure, high frequency,
thermally stabilized, electro-optically regulated Hg vapor lamp, which
produces the Hg emission spectrum. Emitted light is collimated (L1) and
projected in two parallel, isolated beams one each through the reference
and sample cells. Absorbance of 253.7nm radiation by Hg0 vapor (derived
from the chemically reduced sample and GLS) occurs only in the sample
cell. P is thereby decreased, relative to P0.

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Light from the cells enter the binocular camera, where both collimated
beams are independently focused (L2) and filtered (F) before reaching the
Charged Coupled Device (CCD) detector. Narrow band 254 +/- 2nm
interference filters (F) remove all radiation but the strong 253.7 nm Hg0
"resonance line" from both the sample (P) and reference (P0) beams. By a
photovoltaic effect, the CCD converts the light beams into electrical signals,
proportional to radiant power (P and P0). These outputs are processed to
yield an electrical signal proportional to optical absorbance (Abs = -log
(P/P0)).

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4.2 Software
The QuickTrace Software operates under a Windows environment. The
QuickTrace software provides complete instrument and autosampler
control. The QuickTrace software also provides a variety of EPA compliant
quality control functions, display features, report generation and diagnostic
routines.

The reader is referred to the separate QuickTrace Mercury Analyzer

Software Manual for a detailed description of the software features,
functions, and operation instructions.

4.3 Preparing Reagents and Calibration Standards

Always use high purity gas, chemicals, acids, water, standards, and clean
glassware for analysis. It may be necessary to acid wash and rinse all
glassware more than once to eliminate contamination for the most sensitive
mode of operation (<20ppt).

Recommended Chemical Concentrations:

Reagent 10%(w/v) SnCl2 in 7%(v/v) HCl

Standards for All instrument calibration standards

Instrument Calibration (Hg2+ ) are prepared in 7%(v/v) HCl
then an aliquot of standard is
treated to the same procedure as a
sample prior to instrument
calibration

Rinse 1%(v/v) HCl/HNO3 trace metal

grade in the Autosampler rinse
reservoir bottle

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NOTE:

HCl media must be used for stock standard preparation! Hg standards in nitric acid
(only) are unstable at ppb levels and below. With 7% HCl media (in glass at room
temperature), the standards are stabilized for weeks at the ppb level, and for several
days at the ppt level. Standards must be 7%(v/v) HCl even after final dilution.

NOTE:

1% HCl/HNO3 rinse prevents carryover contamination from high samples and

standards to subsequent low samples. (Deionized water (alone), as rinse does not
ensure this.)

NOTE:

The CETAC QuickTrace M-6100 Mercury Analyzer measures inorganic mercury

(free Hg2+ or HgCl2, which is subject to efficient stannous chloride reduction in the
QuickTrace M-6100 tubing reactor). Inorganic mercury standard solutions are used
for instrument calibration. If insoluble mercury, bound mercury, or
organomercurials are present in samples, an appropriate sample
dissolution/digestion procedure will have to be employed to convert these forms to
free inorganic Hg2+ or HgCl2, prior to analysis with the QuickTrace M-6100. If it is
desired to confirm the oxidative digestion procedure accuracy (recovery) regarding
organomercurials, then organomercurial standards or appropriate standard reference
materials would have to be carried through the digestion as “process standards”.

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The handling of organomercurial concentrates, which may be used
WARNING
in the preparation of process standards, presents a substantial
(potentially lethal) safety hazard. Only an experienced,
professionally trained organo-metallic chemist, knowledgeable and
skilled specifically in the safe handling of organomercurials (using
approved apparatus and approved protection measures in an
approved facility) should attempt to prepare diluted
organomercurial process standards from concentrates. Always be
sure to obtain and carefully read the MSDS (Material Safety Data
Sheets) before handling organomercurials!

NOTE:

CETAC Technologies assumes no liability for the handling of organomercurial

concentrates or the preparation, handling, or use of diluted organomercurial process
standards.

In most cases, CETAC Technologies recommends that samples be oxidized

following standard, safe, well known, approved sample dissolution or
digestion procedures, and that the QuickTrace M-6100 instrument
calibration standards be prepared only from inorganic mercury
concentrates or diluted from commercially available inorganic mercury
standard solution concentrates. Where possible, the recommended means
of overall process (dissolution/digestion + QuickTrace M-6100 analysis)
validation should be through use of commercially available standard
reference materials (SRM’s) of composition matching (or similar to) the
samples and containing certified, known mercury levels in a concentration
range similar to the samples. (Being by far the safest alternative, this SRM
approach to overall process validation should be used whenever possible,
and is nearly always preferred to preparing diluted process standards from
hazardous organomercurial concentrates!)

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4.4 Carrier Gas Control

The gas control for the QuickTrace M-6100 is through the regulator
controlling the pressure at the gas source. The user adjusts the gas
pressure to achieve a desired flow rate.

Carrier Gas N2 UHP, high purity grade cylinder

(dry, research grade) or Argon, high
purity grade (e.g. liquid dewar boil-
off or cylinder )

Gas Pressure 20-100 psig

Gas Flow Rate 20 - 350 ml/min

Pressure setting (psig) Nominal Flow (sccm)

10 20
20 55
30 95
40 140
60 240
80 295
100 350
120 415
Table 4-1 – M-6100 Carrier Pressure vs. Flow

For exact pressure and flow parameters for your instrument, please consult
the final test documentation that accompanied the instrument.

See Table 4-2 and the QuickTrace M-6100 Mercury Analyzer Software
Manual for a more complete listing of optimal instrument setups.

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4.5 Start-up and Analysis of Samples

Power on the QuickTrace M-6100 and ASX-400 autosampler. Open the
QuickTrace software. The lamp will require about 15 minutes to stabilize.
Other instrument preparation (wetting the GLS, loading standards and
samples, etc.) may be performed during this time.

Once the QuickTrace M-6100 has powered up, check that the 4-channel
peristaltic pump is plugged in. Make sure the pump tubing is installed and
tension is adjusted per Section 3.13. Check also that supply gas is
connected and 60 psig pressure is applied to the unit. This is the pressure
at which we will perform the “Wetting of the GLS”, described below.

The system software controls the peristaltic pump. Ensure that the KMnO4
trap is filled per Section 3.11. The analyst may now operate the QuickTrace
M-6100 to perform analysis of samples. The QuickTrace M-6100 Mercury
Analyzer Software Manual has been developed specifically to assist the
analyst in this task. Refer to this manual to perform the desired analytical
tasks. Once finished, the analyst should place the QuickTrace M-6100
instrument in either Standby (see the QuickTrace M-6100 Mercury
Analyzer Software Manual) or Cold Shutdown condition.

4.5.1 Wetting of the GLS

At the beginning of each day or after any period of pump inactivity and
prior to analysis ensure that the GLS center post is fully wetted.

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11->HG Vapor->12 tube

Pinch the Drain

tube here

GLS
Figure 4-2. Wetting the GLS

Refer to figure 4-2 while reading the procedure below.

1. Disconnect “11Æ
ÆHG VaporÆ
Æ12” tube from the GLS vapor outlet.
2. Set the gas pressure to 60 psig. This should result in a gas flow
of about 240 mL/min.
3. Check that the bottle supplying the ASX-400 rinse station is
filled with clean trace metal grade 1% HCl/HNO3 v/v rinse
solution.
4. Place the reagent sipper in a beaker of DI water.
5. Turn peristaltic pump on.
6. Clamp the pump quick release mechanisms.
7. Using the quick-release mechanisms, fully release the clamp
tension on channels 1 & 2 (drain channels) of the peristaltic
pump.
8. Pinch the drain tube as shown in figure 4-2.

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9. With the drain pump tubes unclamped, the GLS should begin to
fill with liquid. Once the liquid level rises, gas will bubble
through it.
10. Allow the GLS to fill until a gas bubble propels a "meniscus"
upward to wet the post all along its length, including its top.
(THE POST IS NOW WETTED)
11. When this happens, re-engage the quick-release clamps on the
drain pump tubes and un-pinch the drain line.
With the drain tube clamps properly re-engaged and the
pump running, the liquid will begin draining.
12. Once the GLS has "emptied", leave the pump running (keep
liquid flowing), reconnect “11Æ
ÆHG VaporÆÆ12” tube to the GLS
vapor outlet.
13. Place reagent sipper in the SnCl2.
14. The post is now wetted and the QuickTrace M-6100 is ready to
run samples.

Note:

Concentration ranges greater than 20 ppb may require a higher percent acid in the
rinse solution. A 5% HCl/HNO3 v/v should be sufficient for the highest
concentration mode.

Note:

If you do not want to consume stannous chloride reagent during a "standby"

condition, you may alternatively keep the GLS center post wetted by immersing the
reagent sipper tube in a beaker of deionized water (with the sample sipper tube also
immersed in the ASX-400 rinse station).

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4.6 QuickTrace M-6100 Startup Summary

1. Initiate QuickTrace M-6100 software (if the software was left

open and in standby, open the QuickTrace M-6100 controls and
start the autosampler rinse pump (click pump on and probe
down)).
2. Turn on lamp and initiate the carrier gas flow. A minimum of a
15-minute warm-up time is required.
3. Clean and rinse the 2L rinse bottle with DI water and refill with
trace metal grade 1% HCl / HNO3 solution.
4. Place the autosampler rinse tubing into the rinse bottle.
5. Prepare a fresh 10% SnCl2.H2O w/v 7% HCl v/v solution if old
solution is yellow (oxidized) or precipitated. Prepare only what
you need to complete the calibration and sample run including
all QC checks and spikes. The reagent flow is ≈ 1.5 ml/min.
6. Verify that the sample capillary (inlet insert) is 0.5mm above
the Gas/liquid separator (GLS) center post.
7. Open vents on waste container.
8. Inspect peristaltic pump tubing for wear and flat spots (replace
if necessary). Place the peristaltic pump tubing in their
appropriate holder clips on the tubing bridge. Do not lock
clamps at this time.
9. Place the reagent capillary in a beaker of DI water.
10. Lock down the peristaltic shoe clamps.
11. Inspect liquid flows. The GLS drain should be flowing smoothly
with no build up or pulsing of liquid. The waste line from the
peristaltic pump to the waste container should be liquid/gas
etc… with no vibration. If this is not the case upon inspection,
stop immediately and change GLS drain line and or waste line.
12. Wet the GLS center post per Section 4.5.
13. Inspect the rinse station for a convex liquid bubble adhering to
the sample probe. If this is not the case, change the rinse pump
peristaltic tubing.

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14. Open the appropriate worksheet (see QuickTrace M-6100
software manual) and set the gas pressure to match the method.
15. Record lamp current in a daily instrument logbook.
16. Zero the QuickTrace M-6100 using the auto zero.
17. Peak profile the high standard and verify baseline and sample
integration times. Record µAbs and concentration of the peak
profile standard in a daily instrument logbook. Note: This
operation should be performed on the highest standard.
18. Calibrate instrument and analyze samples.

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Typical Results and Settings
RANGE #1: M-6100 PPT <0.01 - 1 ppb Hg
Gas Pressure 20 psig
Peristaltic Pump Speed High
Sample Flow Rate ~ 6 mL/min
Sample Time (for Liquid Uptake or Autosampler "Sip") 50 s
Rinse Time 100 s
Read Delay 65 s
Replicate Read Time 3s
Replicates 4
Baseline Correction Method 2 point (15-25s & 135-145s)

Expected Results: 100 ppt | 7% HCl ~1400 uAbs

Detection Limit (nominal): < 0.010 ppb

Sample Throughput Rate (minutes/sample) 2.5 min/sample
Dryer Cartridge Life 3-6 months

Table 4-2A. PPT Range Settings and Expected Results

Figure 4-3A. Typical Results from PPT Settings.

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RANGE #2: M-6100 PPB 0.1 – 20 ppb Hg

Gas Pressure 30 psig

Peristaltic Pump Speed High
Sample Flow Rate ~6 mL/min
Sample Time (for Liquid Uptake or Autosampler "Sip") 30 s
Rinse Time 90 s
Read Delay 49 s
Replicate Read Time 1.5 s
Replicates 4
Baseline Correction Method 1 point (26-30s)

Expected Results: 10 ppb | 7% HCl ~50,000 uAbs

Detection Limit (nominal): < 0.05 ppb

Sample Throughput Rate (minutes/sample) 2 min/sample
Dryer Cartridge Life 3-6 months

Table 4-2B. PPB Range Settings and Expected Results

Figure 4-3B. Typical Results from PPB Settings.

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4.7 Placing the QuickTrace M-6100 in Standby

Mode
To prolong instrument life, it is not recommended to leave the system
fully on (with lamp lit) overnight, or when not in use. However, for a warm
start the next day, the QuickTrace M-6100 can be placed in Standby Mode
overnight (see QuickTrace Software Manual) without significantly
shortening its life. When analysis is done for the day, rinse with 10% HNO3
for several minutes through the reagent uptake tube. Then rinse with
deionized water through the reagent uptake tube for several minutes.

Note:

Failure to perform this “shutdown rinse” may result in a system clog.

Next, withdraw the reagent uptake tube, and using the QuickTrace M-6100
Software Instrument Control Screen withdraw the Autosampler probe from
the rinse station. Continue pumping until the drain tubing runs fully
empty. Turn off the pump, unclamp all pump tubes and unhook them from
one side of their tubing bridge. Turn off the gas (main supply) and
disconnect the Hg vapor tube from the GLS.

Leave the system power on. The Hg lamp sent with the system has an
operation life of ~5000 hours, but internal optical filter life may be
substantially extended by turning off just the lamp whenever analyses are
not being performed. Leaving the main power on leaves the lamp block
heaters on, and consequently the lamp block remains thermally stable. To
reactivate the instrument to “run” status, simply turn the lamp on again,
re-establish appropriate gas and liquid flows and operate the instrument
normally. The system will be stable and ready to run within 5-10 minutes.

4.8 Cold Shutdown

For a total system shutdown (to cold condition), prepare the pump tubing
as described in Section 4.6 above, and turn off the Hg lamp, gas, ASX-400,
pump, and QuickTrace M-6100 main power. Exit the QuickTrace Software,
shutdown windows, turn off the computer.

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4.9 Summary of QuickTrace M-6100 Shutdown

Shutting down the QuickTrace M-6100 and autosampler.

1. Place the reagent capillary in a beaker of 10% HNO3 and cap the
reagent bottle. Rinse the system for a minimum of ten minutes.
2. Place the reagent capillary in a beaker of DI water and rinse the
system for one minute.
3. Raise sample probe via QuickTrace M-6100 controls.
4. Remove reagent capillary from DI water.
5. Allow the drain and waste lines to run completely dry.
6. Turn off peristaltic pump.
7. Release peristaltic shoe clamps and release the pump tubing from
the tubing bridge.
8. Close vents on waste container.
9. Disconnect GLS exhaust line from GLS.
10. Turn off gas and lamp.
11. If you are going to use the instrument the next day or in the near
future, leave the instrument in this condition. It will then be ready
for a warm start.
12. If you are not going to be using the instrument in the near future
then exit the QuickTrace software and turn off the autosampler and
QuickTrace M-6100.

Note:

Before shutting down the instrument to either Standby or Cold condition, remember
to run 10% HNO3 and deionized water through the SnCl2 reagent lines. This will
clean out any chemicals from the peristaltic pump and sample tubing and prevent
residue encrustation in the Gas - liquid Separator and its drain. Remember to pump
all lines completely dry after rinsing.

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Always remember to release all clamps and unhook the pump tubing from
CAUTION
the peristaltic pump. Failure to release clamps and unhook the tubing
when the pump is off, will cause tube fatigue and lead to poor results (bad
% RSD) when used for analysis the next time.

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5

Maintaining the QuickTrace

M-6100
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Maintaining the QuickTrace M-6100

5. Maintaining the QuickTrace

M-6100

5.1 Daily Maintenance (always check before

analysis)
• Ensure that the Autosampler rinse bottle is rinsed with DI water
and refilled with 1% HCl/HNO3 v/v higher acid concentration
should be used for standards and samples greater than 20ppb. A
5% HCl/HNO3 v/v should be sufficient.

• Ensure that rinse bottle tubes are completely submerged in rinse

solution. The rinse station supply tubing should be at the bottom
of the rinse bottle and the rinse station return tubing should be at
the top of the rinse bottle. This will ensure that the rinse is a true
recirculating rinse. Inspect the rinse station flow and ensure that
the rinse is not removed via the sample probe faster than it is
supplied. Replace the ASX rinse pump tubing periodically for best
performance (see ASX operator’s manual).

• Inspect the sample peristaltic pump tubing for fatigue and wear.
Replace if too worn or fatigued.

• If the pump tubing was left clamped overnight, install new tubing.

• Pre-wet the GLS center post and be sure it remains completely

wet during operation.

• Check that the liquid flows, to and from the GLS, are smooth.
Verify by close inspection the inlet to the GLS center post and
drain exit points.

• Be sure the waste bottle will not overflow during the run.

• Check that the Reagent bottle is sufficiently full for the number of
samples to analyze.

• Check that the SnCl2 is fresh and not precipitated, crystallized,

yellowed, or oxidized or that the small cap on reagent bottle was
left open overnight. Replace if necessary.

• For Autosampler maintenance, see ASX-400 Operator’s Manual.

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5.2 Weekly Maintenance

• Remove the GLS and clean if residue is building up. This is
described later in section 5.10.

• Clean the SnCl2 reagent bottle weekly or before refilling.

• Change the pump tubing if it is too worn, appreciably “flattened”,

or left in place overnight.

• Empty the waste bottle. Cap all Luer fittings to carry this bottle.

• Check the cells and cell windows for cleanliness.

5.3 Monthly Maintenance

• Clean the GLS. See Section 5.10.

• Clean the cells and cell windows. See Sections 5.7 and 5.8.

• Replace the GLS inlet tubing and capillary insert. See Section
5.12.1.

• Replace the GLS drain tube if it is clogged or dirty. This is

described in Section 5.12.2.

• Check that the Nafion® dryer cartridge is still good. A failing

Nafion® cartridge may be indicated by loss of mercury absorbance
sensitivity and an increase in the baseline of more then 1000µabs
during a short run of 30 minutes or less. If the mercury
absorbance for a given standard solution drops to 50% or more of
its original value, change the cartridge. See Section 5.13.

5.4 Yearly Maintenance

• Replace the Nafion® dryer cartridge bi-yearly or as needed (see
Section 5.13). A failing Nafion® cartridge may be indicated by loss
of mercury absorbance sensitivity and an increase in the baseline
of more then 1000µabs during a short run of 30 minutes or less. If

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the mercury absorbance for a given standard solution drops to 50%

or more of its original value, change the cartridge.

• Replace the 2-micron filter (see Figure 3-6).

• Replace the external gas tubing (see section 5.11)

5.5 ASX-400 Yearly Maintenance

• Replace the ASX-400 sample probe.

• Replace the ASX-400 rinse peristaltic pump tubing.

See the ASX-400-Autosampler Operator’s Manual.

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5.6 Removal or Inspection of the Sample Cell

5.6.1 Opening the Optics Access Door

The instrument is shipped with the Optics access door (Figure 5-1)
secured with thumbscrews.

Screws

Optics access door

Figure 5-1. Optics access door of QuickTrace M-6100 Mercury Analyzer.

For continued protection against hazards indicated on the

WARNING
warning labels, always retighten these two metal screw-knobs
securely.

Refer to Figure 5-1. For access to the optics interior, first turn off the
main power. Use a flat-blade screwdriver to loosen the thumbscrews
on the Optics access door.

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Thumbscrews

Cells

Clamps

Figure 5-2. Optical cabinet of QuickTrace M-6100 Mercury Analyzer.

Refer to Figure 5-2. Remove the thumbscrews on the optical cell

clamps.

5.6.2 Removing the Sample Cell

Refer to Figure 5-2 and 5-3. The cells are designed for simple removal
and cleaning. When removing the cells, be careful to not touch the cell
windows at the ends of the optical cells. If the cells and cell windows
are dirty, use a clean foam swab and isopropyl alcohol
(spectrophotometric grade only) to clean the surfaces (see Section 5.7).
If needed, the windows can be taken out by removing the end caps and
the O-rings.

Once the cell clamps have been removed, disconnect the carrier gas
lines from the cell end caps. Remove the cell end caps by holding the
glass cell, pull, and rotate the end cap until it slides off the glass cell.
Repeat this procedure for the reference cell. Inspect and/or clean the
cell and its windows per the instructions in sections 5.7 and 5.8, or
perform tubing maintenance as described in section 5.10.

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5.7 Cleaning the Cell Windows

Refer to Figure 5-3. There are two ways to clean cell windows:

• Quick Exposed Surface Cleaning (without dismantling)

• Dismantling for Total Cleaning

The need for cleaning (or re-cleaning) is determined by close

inspection of the window (D), visible through the hole in the window
cap (A), while maintaining a low-angle total surface reflection of room
light on the window. Any film, fingerprint, dust, or dirt will show up
dramatically against the “white” background of a low-angle surface
reflection of room light from the window.

5.7.1 Quick Exposed Surface Cleaning

Cleaning the exposed surface of the window requires the following: a

clean foam swab, Kimwipes, and a bottle of isopropyl alcohol (use
only spectrophotometric grade).

Note:

Do NOT use cotton swabs. They will leave small bits of lint, which
can offset the absorbance baseline and add a great deal of noise, if
the lint moves or flutters in the optical beam. Use only clean foam
swabs. To pre-clean the foam swab, rinse in alcohol and dry with a
Kimwipes. Do not dip the swab in the alcohol supply (when new,
the swabs may be dirty and contaminate the alcohol supply).
Instead, squirt alcohol onto the swab with a wash-bottle that is for
alcohol only and dry with the Kimwipes. Rinse and only lightly blot
the swab with Kimwipes when cleaning, this will leave the swab
moist with alcohol, which will be enough to clean the cell windows.

Using the pre-cleaned, alcohol-moistened swab, gently swab the

outside of the cell window. Allow to air dry or blow-dry with UHP
Argon or Nitrogen. Re-check the surface reflection to see if the
window is completely clean. If residue, fingerprints, or particles
remain, repeat the process with another pre-cleaned alcohol-
moistened foam swab until the windows are clean. If this quick
procedure fails, it may be necessary to dismantle the assembly for
more rigorous “total” cleaning, as described below.

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Figure 5-3. Cell assembly diagram.

A - Window cap C - Phillips screws E - Cell end cap
B - Window O-ring D - Sapphire windows F - Glass cell

5.7.2 Dismantling for Total Cleaning

Refer again to Figure 5-3. Total cleaning requires a small Phillips

screwdriver, clean Kimwipes, isopropyl alcohol, and a clean plastic
forceps. Carefully pull the cell end caps (E) off the cell (F), using a
twisting motion, next remove the Phillips screws (C) and the window
caps (A). This will allow the sapphire windows to be removed. Grip
the window (D) with the forceps or wear powder free gloves when
cleaning. Squirt the window with alcohol or use an alcohol wetted
foam swab, then rub the surface of the window clean with a Kimwipe.
Rotate the forceps to a different position on the window and repeat the
cleaning. Blow-dry with clean UHP Nitrogen or Argon.

Clean the entire end cap (E) including the O-ring (B) and gas ports
with alcohol. Do not handle the cleaned parts with your fingers; use
clean forceps or powder free gloves. It will be necessary to blow dry
the end cap; gas orifice and fitting with clean gas before assembly. Be
sure not to touch the windows after cleaning.

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5.8 Cell Assembly

Reassemble the sapphire window (D), O-ring (B), and a window
retainer (A) onto the cell end cap (E) with three flat-head Phillips
screws (C), as shown in Figure 5-3. Be sure not to touch the clean O-
ring (B). Handle it instead with clean forceps.

Grip the cell (F) near one end and insert the cell into the open end of
the cell end cap (E) with a pushing twisting motion. From Figure 5-4,
which shows the “open” end, note that each cell end cap has two
imbedded O-rings (A, B). Firmly push (with twisting motion) the cell
into the open end of the cell end cap and continue pushing until both
O-rings (A, B) are fully engaged.

Figure 5-4. Open end of cell end cap.

A - O-ring B - O-ring
Inspect the assembled cell to determine that both O-rings (A, B) are
fully engaged as shown in Figure 5-5. In Figure 5-5, shown without
the window and cell cap, area “C” reveals no O-ring gap. This
indicates that both O-rings A and B of Figure 5-4 are fully engaged.
Figure 5-6, shown with window and cell cap, also reveals no O-ring
gap at point C (the boundary between the cell end (E) and the cell end
cap.

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Figure 5-5. Engaged O-ring. Shown without the window and cell cap.
C - No gap visible

Figure 5-6. Engaged O-ring. Shown with the window and the cell cap.

C - No O-ring visible D - Window O-ring E - Cell

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Note:

The O-ring “D” visible in Figure 5-6 seals against the cell window.

If a O-ring is NOT engaged, as in Figure 5-5, the O-ring “B” figure 5-7
is visible in the gap immediately at the end of the glass cell “E” figure
5-7. This should look, instead like region “C” in Figures 5-5 and 5-6. If
the O-rings are not engaged correctly (as in Figure 5-7), then the
system may drift, and perform poorly. Assemble and attach the
remaining cell end cap to the other end of the glass cell.

Figure 5-7. O-ring NOT engaged.

B - O-ring is visible E - Cell end

An alternate means of checking complete engagement of all O-rings in
both cells is to measure the overall length of the fully assembled cell
with a ruler. If the overall assembled cell length is 8 29/32 inches
(226.5 mm) then both O-rings are engaged, 8 31/32 inches (228 mm)
indicates one O-ring is not engaged, 9 1/32 inches (229.5 mm) indicates
that two O-rings are not engaged (one in each end).

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Note:

The glass tubing is sufficiently thick-walled that there is almost no

danger of breakage (provided you have gripped near the end being
inserted). However, to error on the side of caution, grip the glass
tube with a sufficient thickness of cloth or paper towel to protect
your hands in the unlikely event of glass breakage. Never insert or
try to use a cracked or chipped glass tube.

Once the cell has been completely assembled, with both O-rings fully
engaged, place the cell on a flat surface with both cell end cap “flats”
facing downward. Rotationally adjust the cells until both “flats” are
flat against the surface and parallel with each other. Recheck O-ring
engagement (as above) and re-inspect both windows under low-angle
reflection illumination to verify that no residual dust, lint,
fingerprints, or other smudges exist on the windows. If both windows
are “clean”, attach the appropriate Viton interconnect tubing and
reinstall the cell into the oven.

To reinstall the clean (and/or re-tubed) sample cell, first check that the
two cell holder "flats" are parallel to each other. A simple check will
reveal both cell end cap flats to be completely “tight down” against a
flat surface with no gap visible between the end cap and the flat
surface, when parallel.

Finally, reconnect the tubing and the optical cabinet cover.

5.9 Cleaning the Gas - liquid Separator

Periodically it will be necessary to clean the Gas - liquid Separator
(Figure 4-2). Try pumping 10% HNO3 through the system for 30
minutes continuously, followed by a deionized water rinse. For more
aggressive cleaning, disconnect all tubing from the GLS. Be careful
not to pull hard on the tubing; this can break the glass side arms off.
Instead, use a fingernail to gently work the tubing off the glass arms.

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Retainer
Screw

GLS

Figure 5-8. GLS Removal

Refer to Figure 5-8. Loosen the white plastic retainer screw, and
carefully remove the GLS by rotating the vapor outlet to the front and
slide the GLS down through the clamp and exiting at the clamp
bottom.

Once the GLS is removed, place it in a beaker containing 10% HNO3

v/v in DI water. If an ultrasonic bath is available, place the beaker in
the bath and sonicate for 30 minutes. Otherwise, let the GLS soak for
2 hours in the 10% HNO3. If excessively dirty immerse the GLS in a
mixture of 20 % nitric and 20% sulfuric acid and heat on a hot plate
for several hours or until clean.

Next, rinse with DI water and dry. Reassemble GLS as shown in

section 5-11. Tighten the plastic screw finger tight only.

Hot concentrated acids may cause severe burns, severe fume

inhalation trauma and/or death. They should be handled only
WARNING
by professionally trained chemists, who employs proper safety
precautions and equipment (hoods, goggles, gloves, tongs,
etc.).

5.10 Changing the External Gas Tubing

Once each year, replace the external liquid and gas tubing. To do this,
begin by removing the autosampler, and opening the front door and
Optics access door.

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Next, replace the tubing as shown in Figures 5-9 and 5-10. The
replacement tubes, which are in the external tubing kit, are labeled
and precut to length. See Figure 5-9 for label designations. Match
these numbers and letters with Figure 5-10 and the existing tubing, to
see where each labeled tube should go. It is best to replace one tube at
a time.

In Figure 5-9 connect the number printed on each tube end label (See
“Tubing Label Schedule”) to the same circled number in Figure 5-10
diagram. Refer to Figure 5-10 to see the exact tube routing.

GAS SUPPLY GAS EXHAUST

RESTRICTOR

TUBING LABEL SCHEDULE

1 --->LIQUID MIX---> <---GAS<---9
2 <---LIQUID MIX<--- --->GAS--->10
3 --->DRAIN----> 11 --->HG VAPOR--->12
4 <---DRAIN<---- 13 --->DRY HG VAPOR--->
5 --->GAS SUPPLY---> 14 <---SAMPLE GAS<---
6 <--REFERENCE GAS IN<-- <---EXHAUST<---15
<-REFERENCE GAS OUT<-7 16 <---GAS EXHAUST<---
8 <---GAS<---
SAMPLE REFERENCE
<--DRYER GAS SUPPLY<--5A
CELL CELL 12A<--DRYER GAS IN
20<DRYER EXHAUST-
<--DRYER SUPPLY-17

1/16" o.d. PEEK TUBING (RESTRICTOR)

7
1/8" o.d. SILICON TUBING
1/8" o.d. VITON TUBING

20
1
4

17

14 14

2
BULKHEAD

11
12
NAFION
GAS LIQUID DRYER
SEPARATOR

Figure 5-9. Tubing Diagram and Connection Table.

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To remove an old tube from a plastic connector, grip it near its

connector and pull firmly. For glassware, it is better to slit the old
tube with a razor blade or sharp knife, before removing. Alternatively,
you may use the edge of a fingernail to ease the tube off its glass arm.

A simple way to avoid making wrong connections is to remove only one

tube at a time, and replace this tube with the appropriate, labeled new
one, before proceeding to the next tube.

Drying cartridges are replaced as assemblies (tubing already

attached).

17
1
7
14 14 2
4

12
11
20
3

Figure 5-10. Tube routing.

When finished, be sure no tubing is pinched when the covers are

replaced.

Replace the Tygon drain waste as described in Chapter 3 installation.

Sample in and drain lines need to be replaced monthly, and Viton gas
lines need replacement annually. A tubing kit is available from
CETAC with the correct labeled tubing included, pre-cut to correct
length. To replace the tubing follow the instructions included with the
kit, or in the section above.

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Note:

Do not use waste tubing other than that provided by CETAC. The
ID and length (3 feet) of the drain tube are optimized for maximum
system stability, and should not be altered. Other tubes are
similarly optimized and substitutions/alterations should not be
made.

5.11 Retubing the Gas - liquid Separator

This procedure should be followed about once a month, unless the
samples are excessively "dirty", in which case the procedure should be
followed more often, as needed.

5.11.1 GLS Inlet

Refer to Figures 5-11. Note tubing routing and then remove all
tubing, drain sleeve (J), inlet capillary (C) and silicone sleeve (D) from
the GLS using the same
procedure as for Viton tubing
above.

A – Liquid mix tube

B - Capillary heat-shrink
C - Teflon capillary
D - Silicone inlet sleeve
E - Sample inlet guide
F - Hg vapor outlet
G - Frosted center post
H - Carrier gas inlet
I - Teflon Drain tubing
J - Silicone drain sleeve

Figure 5-11. Assembled gas - liquid separator.

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Select a new translucent white silicone inlet sleeve (D), and push it
down over the glass sample inlet guide (E) until ≈ 6mm (1/4 inch) of
silicone tubing protrudes above the top of the glass inlet guide (E).

Select a replacement GLS Teflon inlet capillary assembly, (C).

Carefully direct the capillary end of the insert into the top protruding
end of the silicone tube (D), and GENTLY push "straight" down.

The capillary insert (C) should go down inside the inlet guide (E).
Continue pushing gently downward until the exposed capillary end (C)
protrudes below the glass guide (E). Stop pushing when the bottom
edge of the capillary is about 0.5 mm (range of 0.3 - 0.6 mm) above the
top of the GLS frosted center post (G). The two parts should never
touch! Finally, select a replacement liquid mix tube (A). Carefully
slide the end of the Viton liquid inlet tube labeled "2 <-- Liq. Mix <--"
onto the protruding upper end (yellow heat-shrink, B) of the GLS inlet
insert assembly. Continuously watch the lower end of the insert, to be
sure that it’s position does not change. Finally, check that the lower
end of the insert is still spaced 0.3 - 0.6 mm above the frosted center
post (G).

Install the assembled GLS into its holder on the front of the analyzer
and gently tighten the GLS screw clamp (Figure 5-8) Do not over-
tighten, or the GLS may crack. Connect the drain tube and route the
drain and liquid mix tubes in their appropriate tubing clamps. The
above procedure may be done with the GLS in its holder, if caution is
used so the fragile glass ports are not broken.

5.11.2 GLS Drain

Select a new GLS drain tube. Prior to installation, the Teflon drain
tube should be pushed all the way into the silicone drain tube-sleeve.
Do not kink the Teflon drain tube. To install, line up the end of the
assembly against the glass drain and push. Refer again to Figure 5-
11. The silicone tube-sleeve (J) should automatically slide over the
outside of the glass tube, and the Teflon drain tube (I) should slide
inside the glass drain tube as seen in Figure 5-11. Keep pushing until
the Teflon tube is approximately flush with the interior wall curvature
of the GLS, or about 2 mm withdrawn from this point.

Inspect the drain area closely. If the liquid pulsates or segments

immediately prior to the Teflon drain tube end, then try a different
position for this tube end. Try it further inserted (about 1 mm into the
chamber), or try it with less insertion (several mm withdrawn from
the chamber). Select the position that eliminates or minimizes
segmentation and/or pulsation of the flow at the entry point of the
Teflon insert. A steady, high-speed stream of tiny bubbles should form

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within the Teflon drain tube, and larger bubble segments should
emerge from the remote end, where a longer silicone tube is attached.

5.13 Replacing the Nafion® Dryer Cartridge

Replace this cartridge if mercury absorbance diminishes to less than
50% of original value. Refer to Figures 5-9, 5-10, 5-11, and 5-12, which
show a replacement Nafion® cartridge and its installation.

1 Open the instrument front door for access to the dryer

cartridge.
2 To remove the old Nafion® Dryer cartridge, refer to Figures 5-
9, 5-10 and 5-11. Disconnect the following tubes: “11>Hg
Vapor>12” from the GLS arm (11), “>Sample Gas>14” from the
bulkhead (14), and “<Dryer Supply<17”, from the bulkhead
(17).
3 Carefully unhook the remaining Nafion® dryer tube,
“20<Dryer Exhaust” from the clips on the side of the
instrument. Detach the Nafion® dryer from the two black
clamps (Figure 5-10); pull cartridge forward, and set aside.
4 Install a new Nafion® Dryer cartridge and reattach tubes
described above. (When reconnecting Luer lok fittings, be
careful not to kink the tubing, which could cause gas flow
constriction.) Remember to route the tube 20 (“20<Dryer
Exhaust) up through the cabinet cover cut out.

®
Figure 5-12. Nafion Cartridge.

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5.14 GLS Overflow Recovery

Observation of a full or overflowing GLS, absorbance over-range, loss
of gas flow or liquid in the sample cell may indicate a GLS overflow
accident. This could happen if the sample probe is left in the park
position for an extended period and rinse siphons into the GLS. The
sample probe, when not in use should not be submerged in the rinse
station. In addition, during operation an overflow might occur. The
latter could occur if the GLS drain outlet-tubing clogs from non-
filtered digested samples during unattended operation. In addition, it
may occur if the waste pump tubes fail, or the clamp tension is too
loose and or not clamped. When any of the above symptoms occur,
liquid may have overflowed the Nafion® dryer cartridge into the
optical sample cell, and possibly beyond.

If the overflow is discovered quickly, it is possible that the Nafion®

dryer can be cleaned and dried (see step 11) before the membrane
pores become saturated and enlarged, which render the dryer useless.

Follow the steps below to correct the problem and bring the
instrument performance back to normal. Also, refer to section 5.7.2.

1 Shut off the instrument main power and unplug the

QuickTrace M-6100.

2 Open the optical access panel. Inspect the sample cell (in
place) and judge whether any liquid is likely to have passed
through the sample cell to the "gas exhaust".

3 Remove the sample cell, GLS, and Nafion® cartridge (with all
tubing still attached). Place all parts on a clean lab cloth (or
equiv.) on the lab bench.

4 Dismantle the sample cell completely. See Sections 5.7.2.

Do NOT remove the cell window blocks over the optical rail if the cell is
CAUTION
wet or full of water. Do this instead outside the instrument to avoid
spillage onto the optical components.

5 Dump out all water and brine from the sample cell glass
tube.

6 Rinse the sample cell glass tube with deionized water and
oven dry. Alternatively, dry by rinsing with alcohol
(recommended spectophotometric isopropyl alcohol
(isopropanol)) and blowing dry with clean air or nitrogen.

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7 Rinse and dry all remaining cell holder parts, fittings and
transfer tubing by steps similar to 5 and 6. However, do not
oven dry; use the alcohol rinse/blow-dry procedure, instead.
Inspect closely to be sure all water, and/or all residual
alcohol are completely eliminated from all fittings, tubes,
parts, and gas ports.

8 Clean the sapphire window first with water and then as

described in Section 5.7.2.

9 Reassemble the window and cell end caps. Handle the

window with clean forceps or hold by the edge with
fingertips while wearing cloves (verify cleanliness by
inspection with low-angle room light reflection).

10 Install the glass tube into the cell end caps, and seat firmly to
fully engage both O-rings.

11 For Nafion® dryer cartridges that have gotten wet, if not

already disconnected, disconnect the cartridge “sample gas”
from sample cell. Attach a 10mL Lure lock syringe filled with
DI water to tube 14 and gently push the water through the
Nafion® dryer cartridge. The water will exit through the
cartridge at tube 11 (figure 5-12, tube numbered 11). Hold
tube 11 so it is positioned over an empty beaker (do not pull
on tube 11 it may disconnect from the cartridge and render it
useless). Reconnect tube 11 to the GLS. Turn on the
QuickTrace M-6100 and initiate the software. Next, adjust
carrier gas pressure to 20 psig, and allow GLS and cartridge
to blow dry for one hour with flowing gas. Be sure to engage
all peristaltic pump tube clamps before initiating gas flow
(otherwise the gases will leak out the pump tubing and
bypass the Nafion® dryer cartridge).

12 Turn off gas! Reattach cartridge sample outlet tube to the

sample cell and reinstall the sample cell into the QuickTrace
M-6100, close front door, and reattach all tubes except for the
final tube end labeled “20Å
ÅGAS EXHAUSTÅ Å”.

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Note:

More than likely, water saturation of the Nafion® Dryer will

destroy it, making replacement necessary. However, if the
overflow accident is quickly caught, cleaning and drying the
Nafion® membrane immediately (per above procedures) may save
it.

13 Determine whether any rinse solution (acidic stannous

chloride dissolved in water) got past the sample cell (during
the original accident), and into any portion of the remaining
gas exhaust lines and KMnO4 trap. Determine this by
dismantling all fittings "en route" and inspecting for the
presence of any liquid or salt encrustation in any of the
fittings or tube ends. Especially check the dark purple
potassium permanganate powder to see if it is wet and/or no
longer "free flowing" in any part of the trap tube.

If no undesirable condition is found in the above plumbing

inspection, reconnect all the system plumbing and check the
gas flow. Be sure all peristaltic pump tubes are engaged by
their clamps before checking gas flow (otherwise the gases
will leak out the pump tubing and bypass the flowmeter).

If ANY undesirable condition was found during the above

plumbing inspection proceed to step 14. Otherwise, skip to
step 25.

14 Remove the potassium permanganate mercury trap from the

rear of the instrument. If it is completely dry, simply set it
aside. If the vapor trap is wet, empty the KMnO4 and
dismantle the trap. Remove the glass wool plugs; rinse all
parts, fittings and tubes with deionized water and then
Hydroxylamine Hydrochloride. The Hydroxylamine
Hydrochloride will clean any remaining purple color from
the vapor trap. Dry by means of rinsing with alcohol and
blowing dry with clean air or nitrogen. Reinstall loose glass
wool plugs into the endcaps, install one cap, and refill tube
body with potassium permanganate powder (crystals).
Install the remaining end cap and set the trap aside. Do not
reinstall the permanganate trap on the QuickTrace M-6100
instrument at this time.

15 It is still necessary to rinse residual acidic stannous chloride

brine out of remaining internal gas exhaust tubing. Refer to
Figures 5-9 and 5-10. Locate the sample cell exit. Disconnect
the exhaust tube at the sample cell.

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16 Disconnect the “liquid mix” at the tee on the output side of

the peripump. Connect the exhaust tube to this tee.

17 Place a waste receptacle (>100 mL) immediately under the

"gas exhaust" fitting on the rear of the instrument.
Alternatively, use the appropriate Lure fittings and hook
another transfer tube from the rear gas exhaust fitting to the
drain bottle on the floor.

18 Pump 100mL of deionized water through the exhaust line,

until it all passes through to the waste collection receptacle.
Refer to the QuickTrace M-6100 Mercury Analyzer Software
Manual for use of the QuickTrace M-6100 Instrument
Controls to place the autosampler sample probe in 50mL
tubes of deionized water located in standard positions. This
will wash all residual perchlorate salt encrustation and/or
acidic stannous chloride brine out of the internal gas
exhaust lines and fittings.

19 Using QuickTrace M-6100 Instrument Controls, lift the

autosampler sipper tube out of the deionized water tube and
allow the peristaltic pump to push air through the exhaust
tube, until no more water enters the waste receptacle.

20 Reconnect the exhaust tube to the sample cell exit.

Reconnect the liquid mix line to the tee on the outlet sdie of
peripump channels 3 & 4.

21 Reinstall all covers, close all doors.

22 Initiate a reasonable gas flow, then pump rinse solution

through the GLS continuously, and let the system "purge",
"dry", and thermally stabilize for a period of 90 minutes.

23 Reinstall the permanganate trap onto the back of the

instrument.

24 Operate instrument normally.

5.15 Replacing the Hg Lamp Bulb

The effect of lamp current on data quality (absorbance and noise) is
minimal over the range 6-13 mA. When a lamp is new, the normal
operating lamp current is 6.5 – 8.5 mA. As the lamp ages, the lamp
current will automatically adjust to maintain constant emission
intensity reaching the EOFM filter/detector.

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Detector Cover

EOFM block
Lamp Block
Optical Rail
Detector

Camera Block

Lamp Cover

Figure 5-13. M-6100 Optical Rail.

Use the QuickTrace M-6100 Software to check the lamp current. Wait
until the lamp current reaches 15 mA to order a new lamp. At this
point, use a dentist mirror and flashlight to check that the EOFM
filter is not "smudged" (refer to Figure 5-13). If it is clean, order a
replacement lamp. If the EOFM filter, is dirty, clean in place using the
cell cleaning procedure. After cleaning, recheck the lamp current.
Install the new lamp when the current of the old lamp reaches 15 mA,
or if you need greater absorbance sensitivity than the old “high
current” lamp can provide.

To change the bulb, turn off the main power, unplug the QuickTrace
M-6100 completely. Disconnect all power and communication cables
and cords to the ASX 400. Remove the ASX 400 from atop the
QuickTrace M-6100 and set the ASX 400 to one of the sides. Remove
the cabinet screws from the electrical cabinet cover of the QuickTrace
M-6100 and remove the cover. Allow the instrument to cool five
minutes. Locate the "heavy" yellow/orange colored lamp cord, on the
left-hand side of the cabinet interior. Trace the cord backward and
unplug it from the Lamp Controller Board. On the top surface of the
lamp block, push the edge of the gray foam toward the left side of the
instrument. Under the edge of this foam is a small "Allen" set screw.
Insert a 0.050 inch Allen wrench into the setscrew head and loosen the
screw.

Grab the old bulb where it attaches to its yellow cord and pull it
towards the right. The bulb will slide out easily. Clean the new bulb
by wiping clean with a Kimwipe or optical tissue moistened with high
purity (spectrophotometric grade) isopropanol, and allow to air dry (or
blow dry with clean gas). Do not touch the bulb face, once it is clean.

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Holding it by the base, carefully insert the bulb into the lamp block
until it stops. Rotate the bulb base until the scratch mark scribed on
the lamp body faces upward and lines up exactly with a matching
scratch mark on the lamp block housing. This scratch mark may be an
arrow or a date on the yellow power cord. Hold this position carefully
while tightening the Allen set screw. Check that the two scratch
marks match up after the setscrew has been tightened. Plug the
yellow lamp cord into the Lamp Controller Board. This plug only
inserts one way into the socket. Re-install the cabinet cover and
screws, and reposition the ASX 400.

Turn on the unit; allow a 15-minute warm-up. Check the lamp

current on the QuickTrace M-6100 instrument controls menu. If the
current is not in the range 6 – 8.5 mA, call CETAC Service. If the
lamp current is in the range of 6 – 8.5 mA, operate the instrument
normally.

84
6

Troubleshooting the
QuickTrace M-6100
 QuickTrace M-6100 Mercury Analyzer Operator’s Manual
Troubleshooting the QuickTrace M-6100

6. Trouble-shooting the QuickTrace

M-6100

6.1 Cannot Zero Instrument

Perform the following steps:

1 Check that the Hg lamp is on in the software and that the

main power switch on the back of the instrument is in the on
position (up). Verify the yellow light on the front panel is on.

2 Be sure instrument is fully warmed up. 15 minutes is long

enough.

3 Check that both cells (sample & reference) and cell end caps
are clean and "dry" (no liquid or dried stannous chloride
obstructing the gas flow or the optical beam. If so, see Section
5.7).

4 Check that both cell windows are clean (See Section 5.6.2).

6.2 Drifting Baseline

The system might not be thermally stable because of insufficient warm
up time. Wait longer.

• Check that gas pressures are stable and correct. Variable gas flow
can cause the baseline to drift. Check that no stannous chloride
encrustation exists in gas lines/fittings after a GLS overflow
accident. See Section 5.6.2.

• Check that the gas hoses are not pinched.

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• Check that the lamp block heater works. The lamp block should be
hot (50°C) to touch. Turn the lamp power off. Remove lamp housing
cover and touch the lamp block momentarily to verify that it is hot.

• With the Hg lamp off, check that the EOFM filter is not dirty
(inspect it with a dentist’s mirror and low angle flashlight).

• Check that the lamp current is not too high using the QuickTrace M-
6100 Instrument Controls. High current indicates a worn-out lamp,
if all the windows and optics are clean.

• Replace the Nafion® dryer cartridge.

6.3 Low Absorbance or No Mercury Response

Check that the Hg lamp is on.

Check all liquid uptake rates and gas flow. If there is no liquid or gas
flow, see Section 6.5 below.

• Check that the reagent tube is in the reagent bottle.

• Check that SnCl2 is active, not empty, not oxidized or precipitated.

• Check that standards have the correct Hg concentrations in them.

• Check the liquid lines for kinks or clogs.

• Check that standards have 7% HCl in them.

• Check the gas flow at the GLS outlet.

• Check the gas flow at the Sample Cell outlet.

• Check that the gas flow at the KMnO4 trap outlet; does not drop in
pressure or flow, this indicates an upstream block or a leak.

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• Check all plumbing connections for correct location and proper seal.

• Replace the Nafion® dryer cartridge.

• Mechanically block the sample beam optical path (e.g. with a

business card) and see if absorbance goes full scale (≥ 400,000 µabs).

• Reboot the system: shut down the software, and power down the
QuickTrace M-6100 and ASX-400. Restart, and check the signal.

6.4 No Liquid or Gas Flow

6.4.1 If No Sample or Rinse Flow

• Increase the tension on the sample pump tubing to start flow.

• Be sure the sample, SnCl2, and “Liq. Mix” tubes are not pinched off
anywhere and restricting flow.

• Check especially that neither tube is pinched under the auto-

sampler foot.

• Check that the rinse station is filled with 1% HCl/HNO3 v/v.

• Check to ensure all pump tubing is centered in clamps.

• Check for clogs in sample tubing.

• Check for kinks in the ASX-400 sample probe and sipper tube.

• Check for excessive pump tubing wear. Replace if needed.

6.4.2 If No SnCl2 Flow

• Increase tension on the reagent pump tubing to start flow.

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• Check to see that no precipitate has formed and clogged the reagent
sipper and/or pump tubing.

• Check for excessive pump tubing wear. Replace if needed.

6.4.3 If No Drain Flow

• Increase tension on the drain pump tubing to start flow.

• Check that there is no clogging of the drain outlet tubing of the Gas-
Liquid Separator. If clogged, clean or replace the drain outlet tubing.

• Be sure the drain tube is not pinched off and restricting flow. Check
especially that it is not pinched under the auto-sampler foot.

• Check that the vent port on the waste bottle is open, and that the
bottle is not overflowing.

6.4.4 No Gas Flow or Low Gas Flow

• Check that the in-line gas filter is not clogged. Remove the threaded
connection downstream from the filter and check for gas flow at the
filter outlet.

• Check that all gas supply lines are connected correctly.

• Check that no gas tube is kinked or pinched.

• Be sure that the KMnO4 trap is not packed too tightly (with either
the glass wool plugs or the reagent crystals) and restricting flow.
Repack if too tight.

• Check for leaks/clogs throughout the gas system, especially after a

GLS overflow accident. Check flow after each fitting/component to
isolate the bad section.

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6.5 Double Peak With Low Absorbance

This may indicate a problem with not enough (or none at all) reagent
(stannous chloride) uptake. Check the following items:

• The reagent sipper tube is in the reagent bottle (rather than sitting
in a deionized water container or loose in air).

• There is liquid in the reagent bottle.

• The sipper tube is submerged below the liquid level.

• The liquid is 10% stannous chloride solution in 7% HCl.

• The reagent is not "old", precipitated, yellowed, or otherwise

oxidized (for example, by leaving the bottle open overnight).

• There is no clog, kink, pinch, or other obstruction in the reagent

tubing pathway.

• The reagent liquid uptake rate is at least 1.5 mL/min at 50% pump
speed.

• The ASX-400 sipper tube is the right size, no longer than 3.5 feet
and no smaller than 1.0mm i.d.

• The sample uptake is at least 4 mL/min.

• The ASX-400 probe, reagent sipper tube, QuickTrace M-6100 mixing

tee and GLS liquid/mix capillary inlet is not under pressure from a
partial clog.

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6.6 Poor Reproducibility

• Always be sure to matrix match standards and samples as closely as
possible (excluding the 7% HCl in the standards), and rinse solution
should also be 1% HCl/HNO3.

• Inspect the liquid flow into and out of the Gas-Liquid Separator. If
either the sample in or waste out is pulsing, adjust the clamp
tension on the corresponding tubing in the peristaltic pump to
smooth out flows. If unable to stop the pulsing, check to see if the
pump tubing is worn out. If so, replace the pump tubing. Be sure to
check all the pump tubes.

• Check that the center post is fully “wet”. If partially dry anywhere
on post surface, wet the post see section 4.

• Check to see if the reagent tube is in the reagent bottle.

• Ensure that the stannous chloride has not been emptied or oxidized.
Old SnCl2 can lead to poor results. Replace if yellow, precipitated, or
just too old.

• Ensure that the ASX-400 rinse station and rinse bottle are filled
with 1% HCl/HNO3.

• Inspect both cell windows for fingerprints, films, or debris. If dirty,

clean the windows following the procedure outlined in Section 5.7.

• Check that gas pressure to the QuickTrace M-6100 is 20-100 psig.

• Check the output gas flow after the KMnO4 gas trap with a flow
meter (to check this flow, all pump tubes must be clamped or
plugged). This gas flow should be the same as set in the software.
Check all the seals and recalibrate if necessary. Note calibration
and flow stability.

• Check the gas flow at the GLS exit.

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• Check the gas flow at the Sample Cell exit.

• Check that the optimal instrument settings are employed. See the
QuickTrace M-6100 Mercury Analyzer Software Manual and chapter
four of this manual for details.

• Check that the peristaltic pump rollers are not severely worn.
Inspect all rollers with tubing removed. Roller facets should not be
“grooved”. All rollers should spin freely when turned by sliding your
thumb quickly across them. None should feel “gritty” or slow in
spinning. Replace the head if any one of the 12 rollers are grooved
or fail to move freely .

• Check that the baseline is not drifting severely (See Section 6.2).

• Check that the raw analog system noise is ≤ 100 µAbs. If not, call
CETAC Support.

6.7 Noisy Baseline

• Check that flows into and out of the Gas-Liquid Separator are not
pulsing. Pulsation indicates improperly adjusted pump clamps.

• Check that gas pressures are correct.

• Be sure the SnCl2 is fresh and not oxidized or precipitated.

• Check that the cell windows are clean.

• Check that the EOFM filter is clean. Turn the Hg lamp off and
check that the EOFM filter is not dirty (inspect it with a dentist’s
mirror and low angle flashlight).

• Check that nothing has been spilled on the binocular camera lenses.
Turn the Hg lamp off and check that the camera lenses are not dirty
(inspect them with a dentist’s mirror and low angle flashlight). Call

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Troubleshooting the QuickTrace M-6100

CETAC Customer Service and Support if the camera lenses are

dirty.

• Check that the lamp current is not excessive (>15 mA). Do this with
the QuickTrace M-6100 Software. For more information see Section
5.

6.8 Bad DL
• Check Low Absorbance. See Sections 6.3 and 6.5.

• Check Noisy baseline. See Section 6.7.

6.9 Sudden Standard Absorbance Rise

During Run
• Check that the rinse bottle has 1% HCl/HNO3.

6.10 Poor Accuracy

• Verify good reproducibility (e.g. ~1 % RSD on standard replicates).

• If reproducibility is poor, see Section 6.6.

• Check that standards contain 7% HCl (v/v).

• Check that samples are properly digested.

• Utilize an appropriate process standard to validate digestion and

container storage.

• Check process (digestion blanks, containers, and rinse solution) for

mercury contamination.

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• Check standard solution accuracy, and all gravimetric/volumetric

process steps and equipment for accuracy and calibration.

• If very low samples are run immediately following high samples or

standards, the rinse time may not have been long enough and the
result may be reading low. (Increase rinse times when sample
and/or standard concentrations are widely spread).

• Be sure that the rinse solution contains 1% HCl/HNO3. If it only

contains deionized water, very low samples (acidified) may read
erroneously high if they immediately follow the high standard or a
high sample, regardless of allocated deionized water rinse time. The
problem is avoided by a 1% HCl/HNO3 solution in the rinse solution
bottle.

94
Glossary
QuickTrace Mercury Analyzer Operator’s Manual
Glossary

Glossary
This manual frequently uses the following terms:
A Amperes, electrical current
AAS Atomic Absorption Spectrometry
Abs Absorbance (-log10 T or 2-LOG10 %T)
ADC or A/D Analog-to-digital converter
ADX-500 Optional Auto-Dilutor accessory
ASX-500 The ASX-500, Model 510 Auto Sampler
Bar Unit of pressure. 1 bar = 100 kPa ≈ 14.5 psi
Ar Argon carrier gas, chemical formula
CH3HgCl Methyl mercuric chloride (or “methyl mercury”),
chemical formula of a common organo-mercurial
CLP Contract Laboratory Protocol (analysis protocol of U.S.
EPA)
cm Centimeter (10-2 meter), unit of length
Cold Vapor Direct Atomic Absorption Spectrometric analysis (at
Direct AAS 253.652 nm) of “head-space” gas from a stannous
or CVAAS chloride or stannous sulfate reactor using neither
flame, nor plasma, nor furnace nor any other
electro-thermal atomizer. CVAAS works only for
the element mercury (Hg)
DBA Doing Business As
Dia. Diameter
DL Detection limit. Smallest statistically detectable
concentration, where the absorbance, Abs (produced
by that concentration), equals 3 times the standard
deviation σ of the blank Abs
DSP Digital Signal Processor

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Glossary

ea. Each
EOFM Electro-Optic Feedback Module; used to stabilize the Hg
lamp
EPA U.S. Environmental Protection Agency
EPA-245.1 The standard EPA method of water quality analysis for
measuring mercury (Hg)
ETFE Ethylenetetrafluoroethylene (Tefzel), a polymeric tubing
material
g Gram, unit of mass or “weight”
GCU Gas Control Unit, sets and regulates carrier gas flow
rate
GLS Gas-Liquid Separator
HCl Hydrochloric Acid, chemical formula
Hg Mercury, chemical symbol
Hg0 Mercury, elemental (reduced) state
Hg2+ Mercuric ion, mercury in +2 (oxidized) state, typically
HgCl2
HgCl2 Mercuric chloride, chemical formula
HNO3 Nitric acid, chemical formula
i.d. Inside diameter
IDL Instrument Detection Limit. DL in ultra-clean, high
purity acid media (e.g. 7% HCl, “Ultrex II” grade).
IDL is generally measured under “favorable”
operating conditions and does not involve sample
digestion or preparation steps. IDL indicates what
the instrument is capable of doing, if not subjected
to contamination, digestion loss, storage loss, or
other sample collection/preparation errors or
limitations
KMnO4 Potassium permanganate, chemical formula of oxidizing
reagent, and Mercury Exhaust Trap agent

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QuickTrace Mercury Analyzer Operator’s Manual
Glossary

L Liter, unit of volume

LED Light-Emitting Diode
QuickTrace Specifically the CETAC Mercury Analyzer instrument
that sits below the ASX-500 Autosampler
QuickTrace Specifically the entire Mercury Analyzer system
including the QuickTrace, ASX-500, Peristaltic
Pump, etc.
mA Milliamperes (10-3 amperes), electrical current
MDL Method Detection Limit; DL measured under actual
reagent purity, sample preparation, and storage
conditions for samples, reagents, and containers in
question. Calibration standards are generally
prepared in the sample media and are carried
through all sample digestion/preparation, storage
and transfer steps, etc., as are samples. In the
presence of significant contamination, small
concentration detectability gets worse and the
actual MDL should be redefined as 1/3 the
contamination, but not less than the statistical
MDL!
mL Milliliter (cubic centimeter, cc, 10-3 L), unit of volume
mm Millimeter (10-3 meter), unit of length
MSDS Material Safety Data Sheet specifying chemical hazard
type and level
N2 Nitrogen carrier gas, chemical formula
Nafion® Registered trademark of DuPont (E.I. du Pont de
Nemours and Company), which trademark is
licensed to Perma Pure, Inc. and used (with
permission) herein by SD Acquisition, Inc. DBA
CETAC Technologies. The trademark is descriptive
of DuPont/Perma-Pure’s porous membrane which
passes water vapor, but not Hg vapor
nm Nanometer (10-9 meter), wavelength unit

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Glossary

ng Nanogram (10-9 gram), mass or weight unit

o.d. Outside diameter
P Transmitted radiant power, photon flux at sample
detector (after passing through sample)
P0 Incident radiant power, photon flux at reference
detector (before passing through sample)
PC Personal Computer
PEEK Polyetheretherketone; a machined polymeric
construction material
pg Picograms (10-12 g), mass or weight unit
PID Proportional Integral Differential. Description of a type
of precision heater control device
ppb Parts per billion (ng/mL, 10-9 g/mL, µg/L, 10-6 g/L),
concentration unit
ppm Parts per million (µg/mL, 10-6 g/mL, mg/L, 10-3 g/L),
concentration unit
ppt Parts per trillion (pg/mL, 10-12 g/mL, ng/L, 10-9 g/L),
concentration unit
psi Pounds per square inch. Pressure. 1 psi ≈ 0.068 bar. 1
bar = 100 kPa
psig Pounds per square inch. Gauge reading (above
atmospheric pressure)
PTU Precision-Timed Uptake
Pump or PP Peristaltic Pump
P-P Peak to Peak. A description of how signal noise is
measured (One method)
RMS Root Mean Square. A description of how signal noise is
measured. RMS = 0.707 of peak amplitude (another
method), approximately one standard deviation unit

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Glossary

RSD Relative Standard Deviation. A measure of data

precision or reproducibility
SCR Stannous Chloride Reactor
Sn Tin, chemical symbol. Typically as SnCl2 reagent
SnCl2 Stannous chloride, chemical formula of reducing agent
SRM Standard Reference Material, containing a certified,
known mercury level
T Transmittance (P/P0), often %T or percent transmittance
(P/P0 x 100%)
TC “To Contain” Designation of a type of volumetric flask
calibrated to accurately contain a specified volume
of liquid
TD “To Deliver” Designation of a type of volumetric flask or
pipet calibrated to accurately deliver a specified
volume of liquid
UHP Ultra High Purity
UV Ultraviolet; short wavelength region of spectrum below
370 nm (e.g. 253.7 nm)
VAC Volts Alternating Current
VDC Volts Direct Current
XS A substantial concentration “excess” of one chemical
reactant (over another)
µg Micro-gram (10-6 g), unit of mass or weight
µL Micro-liter (10-6 L), unit of volume
µAbs Micro-absorbance units. (10-6 Abs)

100
M6100 Spare Parts
M-6100 SPARE PARTS

SP 6094
ONE YEAR CONSUMABLE PACK

SP 5606
Replaceable O-RING kit

SP 5705A

SAMPLE / DRAIN TUBING

(12 EACH)

SP 5705B

REAGENT TUBING
(12 EACH)

SP 6037
Kit, gas exhaust fittings

SP 6036

KIT PERI PUMP FITTINGS

102
 M-6100 SPARE PARTS

SP 5653

HG TRAP

SP 5558
KIT, FOAM TIP SWABS
(10 EACH)

SP 5603

REPLACEMENT HG LAMP

SP 5894

NAFION CARTRIDGE REPLACEMENT

SP 6155

NAFION CARTRIDGE REPLACEMENT

ECONOMY PACK
(5 EACH)

X5

103
M-6100 SPARE PARTS

SP 6033

SAMPLE PROBE 1.0mm

SP 5710

TWO MICRON GAS FILTER

SP 5580

FILTER ASSEMBLY FAN KIT

SP 5601

GAS LIQUID SEPARATOR

(2 EACH)

SP 5612

GLASS BALLAST TANK

104
 M-6100 SPARE PARTS

SP 5706

WASTE TUBING
(2 EACH)

SP 6042

GLS DRAIN TUBE

(3 EACH)

SP 5949

CELL GAS TUBING KIT

SP 5812

GLS CAPILLARIES REPLACEMENT

(3 EACH)

105
M-6100 SPARE PARTS

SP 5595

RINSE BOTTLE KIT

SP 5593

WASTE BOTTLE KIT

SP 5594

REAGENT BOTTLE KIT

106
 M-6100 SPARE PARTS

SP 5608

CELL WINDOW KIT

SP 5586

COMPLETE REPLACEMENT CELLS

SP 5582

GLASS CELLS

SP 6035

KIT, CELL FITTINGS

107
M-6100 SPARE PARTS

108