BUCHI D-480 User Manual

5 (1)
BUCHI D-480 User Manual

DuMaster D-480

Operation Manual

11593626 en

Imprint

Product Identification:

Operation Manual, DuMaster D-480 11593626 en

BÜCHI Labortechnik AG

Meierseggstrasse 40

Postfach

CH-9230 Flawil 1

E-Mail: quality@buchi.com

Copyright Note

3

Copyright © BÜCHI Labortechnik AG

All rights reserved

This document contains proprietary information of BÜCHI Labortechnik AG. Reprint is prohibited.

Due to continued product development this information may change without notice. The information and intellectual property contained herein is confidential between BÜCHI Labortechnik AG and the client and remains the exclusive property of BÜCHI Labortechnik AG. If you find any problems in the documentation, please report them to us in writing. BÜCHI Labortechnik AG does not warrant that this document is error-free.

No part of this publication may be reproduced, stored in a retrieval system, or transmitted in any form or by any means, electronic, mechanical, photocopying, recording or otherwise without the prior written permission of BÜCHI Labortechnik AG.

Windows®, Windows XP® and Windows 7® are trademarks of Microsoft Corporation.

MS-Excel® und MS-Access® are trademarks of Microsoft Corporation.

Operation Manual D-480

©BÜCH Labortechnik AG

Contents

5

Contents

CHAPTER 1 General

13

Revision history...........................................................................................................................................

14

About this document....................................................................................................................................

15

Display conventions ....................................................................................................................................

16

General information on the operating instructions.......................................................................................

16

CHAPTER 2 Basic security settings

17

Working with the operating instructions.......................................................................................................

18

Representation of safety instructions ..........................................................................................................

18

Instructions for disposal of consumables.....................................................................................................

18

Intended use of the instrument....................................................................................................................

19

Warning: residual risks................................................................................................................................

19

Safety devices in the analyzer.....................................................................................................................

20

Warning signs on the analyzer ....................................................................................................................

22

Warning: changes to the instrument............................................................................................................

23

Warning: unsuitable spare parts and consumables.....................................................................................

23

Required user knowledge and skills............................................................................................................

23

Required personal safety equipment...........................................................................................................

24

Warning notes during operation ..................................................................................................................

24

CHAPTER 3 Product description

29

Analytical characteristics and technical specifications.................................................................................

30

Analytical characteristics..................................................................................................................

31

Technical specifications ...................................................................................................................

31

Instrument design........................................................................................................................................

33

Front view ........................................................................................................................................

34

Furnace section ...............................................................................................................................

35

Rear view .........................................................................................................................................

36

Right side view.................................................................................................................................

37

Left side view ...................................................................................................................................

38

Top view...........................................................................................................................................

39

Peripherals and their function ..........................................................................................................

39

CHAPTER 4 Understanding the instrument and planning its use

41

Layout and mode of functioning ..................................................................................................................

42

Functional units................................................................................................................................

43

The thermal conductivity detector (TCD)..........................................................................................

45

Processes in the instrument during a measurement ...................................................................................

46

Sample insertion and initiation of measurement ..............................................................................

47

Substance digestion and preparation of the reaction gas mixture....................................................

47

Detection of measuring components and evaluation of the measuring signal..................................

48

Formula for determining element concentration of analysis samples(Solids)...................................

48

Basic facts about working with the instrument.............................................................................................

49

Setting device parameters ...............................................................................................................

50

Instrument equipment ......................................................................................................................

51

Background knowledge required for calibration ...............................................................................

52

Calibration curve calculation method criteria....................................................................................

53

Calibration formulae.........................................................................................................................

55

Routine measuring work ..................................................................................................................

56

Formulae for blank value determination and compensation.............................................................

57

Formula for determining the daily factor...........................................................................................

58

Operation Manual D-480

©BÜCH Labortechnik AG

Contents

6

Understanding the operating software.........................................................................................................

59

Basic functions of the operating software.........................................................................................

60

Software user interface ....................................................................................................................

61

Sample view.....................................................................................................................................

62

Combi view ......................................................................................................................................

64

Status view.......................................................................................................................................

67

Right mouse button function ............................................................................................................

69

Data administration and data security .........................................................................................................

71

Laboratory information and management system (LIMS) ................................................................

72

Conditions for operating the LIMS....................................................................................................

72

21 CFR Part 11 functionality ............................................................................................................

73

Versioning ........................................................................................................................................

74

Linking the analyzer and software....................................................................................................

74

CHAPTER 5 Work performed by the system administrator

75

Installing and updating the software ............................................................................................................

76

Configure analyzer ......................................................................................................................................

77

What can you modify in the configuration? ......................................................................................

78

Defining logon timeout .....................................................................................................................

78

Creating new sections......................................................................................................................

79

Defining LIMS export settings .....................................................................................................................

80

LIMS export settings ........................................................................................................................

81

Setting up user administration.....................................................................................................................

82

User administration ..........................................................................................................................

83

Recommendations for user administration.......................................................................................

83

Granting authorizations....................................................................................................................

83

Defining interfaces.......................................................................................................................................

85

Defining the analyzer / PC interface.................................................................................................

86

Defining the LIMS / PC interface......................................................................................................

86

Defining the balance / PC interface..................................................................................................

87

Editing analysis data ...................................................................................................................................

88

When does it make sense to edit analysis data? .............................................................................

89

Limits for modifying analysis data ....................................................................................................

89

Consequences of modifying analysis data.......................................................................................

89

Performing checks.......................................................................................................................................

90

Checking documents for authenticity ...............................................................................................

91

Signing documents...........................................................................................................................

91

Viewing the logbook.........................................................................................................................

92

Working with the database ..........................................................................................................................

93

Database..........................................................................................................................................

94

Administrative work on the database ...............................................................................................

94

Defining the autoexport directory .....................................................................................................

95

Database backup .............................................................................................................................

95

Starting the database backup ..........................................................................................................

96

Reorganize database.......................................................................................................................

96

Reloading an old database file.........................................................................................................

97

Ways of optimizing the use of the analyzer .................................................................................................

98

Optimizing basic instrument settings................................................................................................

99

Optimizing sample data editing ........................................................................................................

99

"Balance" weighing data input program .........................................................................................

100

Optimizing data evaluation.............................................................................................................

101

Performing other administrator tasks.........................................................................................................

102

Modifying the registration...............................................................................................................

103

Printer setup...................................................................................................................................

103

CHAPTER 6 Starting up and shutting down the instrument

105

Setting up and starting up the instrument..................................................................................................

106

Rules for first-time start-up.............................................................................................................

107

Instructions for operating the furnace.............................................................................................

107

Installation site requirements .........................................................................................................

107

Gases and chemicals to be provided .............................................................................................

108

Operation Manual D-480

©BÜCH Labortechnik AG

Contents

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Start-up ..........................................................................................................................................

109

Connecting peripherals ..................................................................................................................

110

Connecting supply lines and waste gas lines.................................................................................

111

Removing the transport protection .................................................................................................

112

Switching on...................................................................................................................................

114

Default instrument settings.............................................................................................................

114

Shutting down the instrument....................................................................................................................

116

Shutting the instrument down for short measuring breaks (standby) .............................................

117

Shutting the instrument down for long measuring breaks (switching off) .......................................

117

Heating up the furnace / checking parameters

118

CHAPTER 7 Using the instrument

119

Measurement settings...............................................................................................................................

120

Defining keywords for blank and conditioning samples..................................................................

121

Viewing list of defined factor, monitor and standard samples ........................................................

121

Defining custom standard substances ...........................................................................................

121

Defining standard substances as factor and monitor samples.......................................................

122

Defining standard substances as calibration samples....................................................................

122

Specifying the computation method for blank value and daily factor..............................................

123

Enabling/disabling acoustic signals................................................................................................

123

Configuring error handling..............................................................................................................

124

Preparing samples ....................................................................................................................................

125

Sample preparation instructions.....................................................................................................

126

Determining sample weight............................................................................................................

126

Showing or hiding the weight window ............................................................................................

127

Packing samples............................................................................................................................

127

Preparing measurement work ...................................................................................................................

129

Software usage rules .....................................................................................................................

130

Starting the operating software ......................................................................................................

130

Showing or hiding the toolbar.........................................................................................................

130

Waking up the instrument ..............................................................................................................

130

Selecting the operating mode ........................................................................................................

131

Viewing method settings ................................................................................................................

131

Defining custom methods...............................................................................................................

131

Defining the Kjeldahl factor ............................................................................................................

132

Copy methods................................................................................................................................

133

Settings for sample input................................................................................................................

133

Importing weighing data.................................................................................................................

134

Prioritizing urgent samples.............................................................................................................

134

Optimizing sleep and wake-up behavior ........................................................................................

135

Performing measurement work .................................................................................................................

136

Values for oxygen dosing...............................................................................................................

137

Performing measurements.............................................................................................................

138

Performing routine measuring work ...............................................................................................

140

Checklist for blank value / conditioning and daily factor measurements ........................................

142

Checklist for real sample measurement.........................................................................................

142

Types of blank value determination and their settings ...................................................................

143

Determining blank values...............................................................................................................

144

Determining the daily factor ...........................................................................................................

145

Stopping continuous analysis.........................................................................................................

147

Preparing measuring data for evaluation...................................................................................................

148

Configuring the sample view ..........................................................................................................

149

Determine measuring units and number of decimal places............................................................

149

Saving the sample view .................................................................................................................

150

Loading a sample view...................................................................................................................

150

Configure statistics view.................................................................................................................

150

Generating statistical data..............................................................................................................

150

Formulae for generating statistical data .........................................................................................

151

Manual peak integration.................................................................................................................

152

Configuring the graph view ............................................................................................................

156

Operation Manual D-480

©BÜCH Labortechnik AG

Contents

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Setting the size of the graph ..........................................................................................................

156

Configure report .............................................................................................................................

157

Display print preview......................................................................................................................

157

Data backup and printing ...............................................................................................................

158

Overview of export and import file formats.....................................................................................

159

Exporting analysis data to MS Excel and viewing ..........................................................................

159

Exporting LIMS data.......................................................................................................................

160

Working with documents ...........................................................................................................................

161

Creating new documents ...............................................................................................................

162

Editing documents..........................................................................................................................

162

Deleting documents .......................................................................................................................

163

Finding documents.........................................................................................................................

163

Copying documents via the clipboard ............................................................................................

164

Importing documents......................................................................................................................

165

Signing documents.........................................................................................................................

165

Checking documents for authenticity .............................................................................................

166

CHAPTER 8 Maintaining the instrument

167

Important information about maintenance.................................................................................................

168

Maintenance work to be performed by the customer .....................................................................

169

Viewing the status of maintenance intervals ..................................................................................

170

Defining maintenance intervals in the software..............................................................................

170

Installing used tubes ......................................................................................................................

171

Preparing and following up maintenance work...............................................................................

171

Conditioning newly installed tubes .................................................................................................

172

Performing the calibration .........................................................................................................................

175

Viewing list of defined factor, monitor and standard samples ........................................................

176

Defining standard substances........................................................................................................

176

Viewing calibration coefficients ......................................................................................................

177

Optimizing instrument condition for calibration...............................................................................

177

Performing the calibration ..............................................................................................................

177

Assessing the calibration curves....................................................................................................

182

Calibration tables.......................................................................................................................................

185

Calibration table for nitrogen calibration.........................................................................................

186

Replacing the ash crucible ........................................................................................................................

187

Purpose and frequency of crucible replacement ............................................................................

188

Removing the ash crucible.............................................................................................................

188

Installing the ash crucible...............................................................................................................

191

Replacing sealing elements ......................................................................................................................

193

When to replace sealing elements .................................................................................................

194

Removing sealing elements from grooves .....................................................................................

195

Ball valve maintenance .............................................................................................................................

196

Removing and dismantling the ball valve.......................................................................................

197

Cleaning, assembling and installing the ball valve. ........................................................................

201

Maintaining the Ni flap and the O2 lance...................................................................................................

205

Purpose and frequency of maintaining the Ni flap and O2 lance ...................................................

206

Removing and cleaning the Ni flap ................................................................................................

206

Installing the Ni flap........................................................................................................................

209

Removing, cleaning and re-installing the O2 lance ........................................................................

210

Removing, cleaning and installing the quartz glass bridge........................................................................

213

Removing the quartz glass bridge..................................................................................................

214

Cleaning and installing the quartz glass bridge..............................................................................

214

Removing, cleaning and installing the carousel ........................................................................................

217

Removing, cleaning and installing the carousel .............................................................................

218

Emptying and filling reaction tubes............................................................................................................

220

Emptying reaction tubes.................................................................................................................

221

Filling the combustion tube ............................................................................................................

222

Filling the post combustion tube.....................................................................................................

223

Filling the reduction tube................................................................................................................

224

Removing/installing and conditioning the reaction tubes...........................................................................

226

Removing the reaction tubes from the furnace ..............................................................................

227

Installing reaction tubes in the furnace and conditioning................................................................

229

Operation Manual D-480

©BÜCH Labortechnik AG

Contents

9

Filling, removing and installing the absorption and drying tubes

...............................................................233

Filling the drying tubes ...................................................................................................................

234

Removing and installing the drying tubes.......................................................................................

236

CHAPTER 9 Repairing the instrument

239

Interpreting PC error messages ................................................................................................................

240

Performing a system test...........................................................................................................................

241

Performing a leak test ...............................................................................................................................

242

Leak test procedure...................................................................................................................................

243

Replacing fuses.........................................................................................................................................

243

What to do after a computer crash ............................................................................................................

247

Reacting to a power failure........................................................................................................................

248

Stopping continuous analysis....................................................................................................................

250

Re-weighing after sample loss ..................................................................................................................

250

Changing the position of the carousel .......................................................................................................

251

Export analysis data for support................................................................................................................

251

CHAPTER 10 Menu and dialog descriptions

253

Dialog descriptions key .............................................................................................................................

254

File menu ..................................................................................................................................................

255

File > New (Command) ..................................................................................................................

256

Select document name (Dialog).....................................................................................................

256

Select version (Dialog)...................................................................................................................

258

Save file as (Dialog).......................................................................................................................

259

File > Delete (Command)...............................................................................................................

260

Comment modification (Dialog)......................................................................................................

260

Sign (Dialog) ..................................................................................................................................

261

Verify digital signature (Dialog) ......................................................................................................

261

Export to LIMS (Dialog)..................................................................................................................

262

Export peak graphics (Dialog)........................................................................................................

263

Configure report (Dialog)................................................................................................................

263

Print (Dialog) ..................................................................................................................................

265

Print preview (Dialog).....................................................................................................................

266

Printer setup (Dialog) .....................................................................................................................

267

Open (Dialog).................................................................................................................................

268

Load balance file (Dialog) ..............................................................................................................

269

Configure backup (Dialog) .............................................................................................................

269

Clean database (Dialog) ................................................................................................................

271

Restore database (Dialog) .............................................................................................................

271

Log in as (Dialog)...........................................................................................................................

272

File > Logoff (Command) ...............................................................................................................

273

File > Exit (Command) ...................................................................................................................

273

File > Export/Import > Create Excel sheet (Command)..................................................................

273

Edit menu ..................................................................................................................................................

274

Edit > Redo (Command) ................................................................................................................

275

Edit > Undo (Command) ................................................................................................................

275

Edit > Cut (Command) ...................................................................................................................

275

Edit > Copy (Command) ................................................................................................................

275

Edit > Paste (Command)................................................................................................................

276

Edit > Insert line (Command) .........................................................................................................

276

Edit > Delete line (Command)........................................................................................................

276

Swap samples (Dialog) ..................................................................................................................

277

Edit > Modify (Command) ..............................................................................................................

277

Set stop tag (Dialog) ......................................................................................................................

278

Select current sample (Dialog).......................................................................................................

278

Set current weighed sample (Dialog) .............................................................................................

279

Edit > Update hole positions (Command) ......................................................................................

279

View menu ................................................................................................................................................

281

View > Toggle (Command) ............................................................................................................

282

Zoom in/out (Dialog).......................................................................................................................

282

Configure view (Dialog)..................................................................................................................

282

Operation Manual D-480

©BÜCH Labortechnik AG

Contents

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Column properties (Dialog) ............................................................................................................

283

Save views (Dialog) .......................................................................................................................

284

Load views (Dialog)........................................................................................................................

285

Delete views (Dialog) .....................................................................................................................

285

View > Gridview > Auto align (Command) .....................................................................................

286

Configure graph view (Dialog)........................................................................................................

286

View > Gaphic > Auto align (Command)........................................................................................

287

Configure statistics view (Dialog) ...................................................................................................

287

View > Statistic > Auto align (Command).......................................................................................

288

Select columns (Dialog) .................................................................................................................

288

System menu ............................................................................................................................................

289

System > Auto run (Command)......................................................................................................

290

System > Single run (Command) ...................................................................................................

290

System > Stop (Command)............................................................................................................

290

System > Auto zero (Command)....................................................................................................

291

System > Wake up (Command) .....................................................................................................

291

Feeding (Dialog).............................................................................................................................

291

Adjust carousel position (Dialog)....................................................................................................

292

Analysis mode (Dialog) ..................................................................................................................

293

Windows menu..........................................................................................................................................

295

Windows > Toolbar / Run-Bar (Command) ....................................................................................

296

Toolbar...........................................................................................................................................

296

Windows > Recent sample (Command).........................................................................................

297

Windows > Status view (Command) ..............................................................................................

297

Weighing window (Dialog)..............................................................................................................

297

Windows > Default layout (Command)...........................................................................................

298

Options menu............................................................................................................................................

299

Maintenance intervals (Dialog).......................................................................................................

300

Replace part (Dialog) .....................................................................................................................

301

Commands for the maintenance of the liquid sampler VLS ...........................................................

302

Leak test (Dialog)...........................................................................................................................

302

Leak test: Test phases (Dialog) .....................................................................................................

303

System test (Dialog).......................................................................................................................

304

Error buffer (Dialog) .......................................................................................................................

306

Error display (Dialog) .....................................................................................................................

306

Options > Diagnostics > Baseline recording (Command)...............................................................

307

Input options (Dialog).....................................................................................................................

307

Standard samples (Dialog).............................................................................................................

308

Keywords (Dialog)..........................................................................................................................

309

Acoustic signals (Dialog)................................................................................................................

310

Configure Calculations (Dialog) .....................................................................................................

310

LIMS settings (Dialog)....................................................................................................................

311

Device parameters (Dialog) ...........................................................................................................

314

Method (Dialog) .............................................................................................................................

315

Error handling (Dialog)...................................................................................................................

316

Sleep / wake-up function (Dialog) ..................................................................................................

317

Monthly logbook (Dialog) ...............................................................................................................

319

Select period (Dialog).....................................................................................................................

320

Device configuration (Dialog) .........................................................................................................

320

Configure key value (Dialog)..........................................................................................................

323

Math menu ................................................................................................................................................

325

Math > Blank values > Calculate (Command)................................................................................

326

Blank values (Dialog) .....................................................................................................................

326

Math. > Factor (Command)............................................................................................................

327

Define type of peak (Dialog)...........................................................................................................

327

Define peak start / end (Dialog) .....................................................................................................

327

Area assignment (Dialog)...............................................................................................................

328

Standard samples display (Dialog).................................................................................................

329

Math. > Recalculate (Command) ...................................................................................................

330

Statistics menu..........................................................................................................................................

331

Statistics > Via names (Command)................................................................................................

332

Statistics > Group (Command).......................................................................................................

332

Statistics > Sort group (Command) ................................................................................................

332

Statistics > Delete group (Command) ............................................................................................

332

Operation Manual D-480

©BÜCH Labortechnik AG

Contents

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Statistics > Clear statistic (Command) ...........................................................................................

332

Statistics > Include/Exclude sample (Command)...........................................................................

333

Statistics > Include/Exclude value (Command)..............................................................................

333

Calibration menu .......................................................................................................................................

334

Calibration coefficients (Dialog) .....................................................................................................

335

Configure calibration (Dialog).........................................................................................................

336

Specify lower and upper calibration range (Dialog)........................................................................

337

Calibration > Next sample (Command) ..........................................................................................

338

Calibration > Previous sample (Command)....................................................................................

338

Calibration > Next (Command).......................................................................................................

338

Calibration > Previous (Command)................................................................................................

338

Help menu.................................................................................................................................................

339

Help > Content (Command) ...........................................................................................................

340

Help > Find (Command).................................................................................................................

340

Help > BÜCHI Labortechnik AG on the WEB (Command).............................................................

340

Product registration (Dialog) ..........................................................................................................

340

Help > About DuMaster (Command)..............................................................................................

341

CHAPTER 11 Appendix

343

Warranty....................................................................................................................................................

344

Warranty of the overall instrument .................................................................................................

345

Warranty on the furnace.................................................................................................................

345

Accessories, spare parts and consumables ..............................................................................................

346

Smallest workable unit ...................................................................................................................

347

Required accessories.....................................................................................................................

347

Optional accessories......................................................................................................................

348

Index

351

Operation Manual D-480

©BÜCH Labortechnik AG

C H A P T E R 1

 

General

 

Purpose

 

This chapter contains general topics of the document.

 

In this chapter

 

Revision history .............................................................................................................................

14

About this document......................................................................................................................

15

Display conventions.......................................................................................................................

16

General information on the operating instructions .........................................................................

16

Operation Manual D-480

©BÜCH Labortechnik AG

1 - General

14

Revision history

List of modifications in this document up to now

Date

Modification

 

 

 

 

Operation Manual D-480

©BÜCH Labortechnik AG

1 - General

15

About this document

Status of the operating instructions

The status of the operating instructions is: 27.08.2013.

Identification number

The operating instructions identification number is: 11593626.

Validity

The operating instructions are valid for all instruments as from serial number: 16091001.

Analyzer

The operating instructions describe the basis type of the instrument D-480 in N operation mode.

Information about the instrument with different equipment and/or operating mode can be found in the variants operating instructions.

Operation Manual D-480

©BÜCH Labortechnik AG

1 - General

16

Display conventions

Before you start using this guide, it is important to understand the terms and typographical conventions used in the documentation. The following kinds of formatting in the text identify special information.

Formatting convention

Type of information

Triangular bullet ()

Step by step procedure. You can follow these instructions to

 

complete a specific task.

Special bold

Items you must select, such as menu options (e. g. File > New),

 

command buttons (e. g. Cancel), or common accentuation.

Italics

Used to emphasize the importance of an item or for variable

 

expressions such as parameters.

CAPITALS

Names of keys on the keyboard, for example, SHIFT, CTRL, or

 

ALT.

KEY+KEY

Key combinations for which the user must press and hold down

 

one key and then press another, for example, CTRL+P, or

 

ALT+F4.

"Quotation marks"

Denote amongst others the names of dialogs in the software, e. g.

 

the "Replace part" dialog.

{Symbolic name}

Denotes a symbolic name, e. g. {Element} stands for the

 

corresponding name of an element.

 

 

General information on the operating instructions

Pictures

The instruments of BÜCHI Labortechnik AG underlie a permanent development and adjustment regarding the optimum parameter settings. This may lead to deviations in terms of picture display of the manual and the current instrument status which are not relevant for the understanding of the instrument operation.

The valid numbers of the parameter settings and/or variables can be found in the current text part. Therefore, numbers in the pictures of software dialogs are mainly replaced by spaces or only reflect examples. They do not reflect the proper, recommended set values.

Reading aids

Subheadings are displayed in the left margin as reading aids. They sum up the content of the particular section and are useful for quick navigation.

Index

An index is given at the end of the operating instructions that helps you locate certain topics more easily. Index entries always refer to the first page of the section in which the index term is found. Therefore, don't be confused if the index term does not appear on the first page but rather on one of the following pages.

Operation Manual D-480

©BÜCH Labortechnik AG

C H A P T E R 2

 

Basic security settings

 

Target group

 

Personnel working with the instrument.

 

Purpose

 

This section describes basic safety rules required to avoid risks for the user of the analyzer.

 

In this chapter

 

Working with the operating instructions.........................................................................................

18

Representation of safety instructions.............................................................................................

18

Instructions for disposal of consumables.......................................................................................

18

Intended use of the instrument ......................................................................................................

19

Warning: residual risks ..................................................................................................................

19

Safety devices in the analyzer.......................................................................................................

20

Warning signs on the analyzer ......................................................................................................

22

Warning: changes to the instrument..............................................................................................

23

Warning: unsuitable spare parts and consumables.......................................................................

23

Required user knowledge and skills ..............................................................................................

23

Required personal safety equipment.............................................................................................

24

Warning notes during operation ....................................................................................................

24

Operation Manual D-480

©BÜCH Labortechnik AG

2 - Basic security settings

18

Working with the operating instructions

Operating the analyzer

Read the operating instructions thoroughly before performing work with the analyzer.

Storing the operating instructions

Store the operating instructions carefully and make sure the instructions are accessible for all relevant personnel.

Passing on the operating instructions

If you pass on the analyzer, always pass on the operating instructions, too.

Representation of safety instructions

Safety signs

This is a safety sign. Instructions with this sign contain warnings about risks of injury and even death. These instructions must always be observed in order to avoid risks.

Risk levels

The safety instructions are categorized according to the following risk levels:

Risk level

Consequences

Probability

Risk

Death / serious injury (irreversible)

high

 

 

 

Warning

Death / serious injury (irreversible)

medium

 

 

 

Caution

Minor injury (reversible)

medium

 

 

 

Caution

Damage to property

possibly

 

 

 

Instructions for disposal of consumables

Rules

Observe the following rules for disposal of consumables:

Dispose of the consumables according to the relevant disposal categories.

Operation Manual D-480

©BÜCH Labortechnik AG

2 - Basic security settings

19

Read the instructions on the individual chemicals in the safety data sheets. The risk notes for individual chemicals can be found in the R-Phrases. Safety advice can be found in the S- Phrases.

Intended use of the instrument

Intended use

This section describes what the instrument is suitable for and what substances may be analyzed with it.

Description of the instrument

The elementary analyzer is an instrument for fully automatic and quantitative analysis of the element N.

Suitable analysis samples

Only samples that can be decomposed in a controlled manner under the method-dependent combustion conditions are suitable for analysis.

Advice on difficult applications

You have the following ways of getting advice on difficult applications:

You will find useful tips in the "Application notes" on the provided CD.

You will find also the "Application notes" section on the www.buchi.com website.

Warning: residual risks

Hot components inside the instrument

During operation, the furnaces inside the instrument heat certain components to very high temperatures. Even after switching off the instrument, these components stay hot for long periods of time that you can suffer serious burns if working inappropriately inside the instrument.

Observe the relevant instructions exactly in order to avoid burns.

Live components inside the instrument

There are live parts (up to 230V) inside the instrument. When you are working on the electrical components, you may suffer electrocution if you do not work properly. Never bring liquids or leak-test spray in the vicinity of live components.

Observe the relevant instructions exactly in order to avoid injuries caused by electrocution.

Unsuitable consumables and spare parts

If you use consumables and spare parts of an unsuitable type and quality, you risk:

Injuries to the operating personnel

Damages to the instrument

Distortion of analysis results

loss of warranty.

Only use original spare parts and original consumables that you have purchased from BÜCHI Labortechnik AG or authorized dealers.

Samples with potential risks

Samples to be analyzed may pose the following risks:

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Contact with the substances may lead to chemical burns or poisoning.

Combustion analysis of larger quantities of the substance may lead to explosions.

These sample substances include:

Aggressive chemicals such as acids or alkaline solutions

Organic solvents

Explosives

Substances that develop toxic or explosive gas mixtures

You are obliged to protect yourself prior to contact with hazardous substances and to reduce the quantity of the substance to a safe amount.

You are also obliged to observe the safety instructions of the chemical manufacturer on the label of the bottle or in the safety data sheets. The safety data sheets contain risk information about a chemical in the R-Phrases and safety information in the S-Phrases.

Safety devices in the analyzer

Note

The analyzer may only be operated if all of the safety devices indicated in this section are in place and in working order.

Gas supply

Gas supply is only possible if the mains switch is switched on and the software is running.

Temperature monitoring

A temperature limiter automatically switches off the instrument in the event of excess temperature inside the instrument. All heating is monitored by an integrated microprocessor controller. All furnaces are automatically shut down in the event of the following malfunctions:

The heating fails to reach setpoint temperature within the set time.

A thermocouple is defective or displays an illegal value.

The set threshold temperature is exceeded.

Instrument casing

The instrument casing comprises the following, as seen from the top left in the picture:

Right side door

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Front door

Left side door

Rear wall

Instrument cover.

The casing separates hot, live parts from the surroundings.

Protective earth conductor

The electrical components of the analyzer are grounded by a protective earth conductor:

The first protective earth conductor is located on the rear wall of the analyzer.

The second protective earth conductor is located outside the cover of the electrical area (arrow).

The third protective earth conductor is located intside the cover of the electrical area (arrow).

If the protective earth conductor connections need to be detached, they must be re-connected correctly when re-assembling.

Waste gas lines

The operator is obliged to connect waste gas lines if the national limits for toxic gases in workplace air are exceeded. The waste gas lines must discharge into the open or into an exhaust hood. The end of the waste gas lines must discharge into the open at a location protected from the wind as pressure fluctuations, e.g. caused by wind, cause detector instabilities.

In addition, the installation room should be well ventilated.

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Warning signs on the analyzer

Warning sign furnace

The following picture shows the warning sign on the furnace heat protection cladding:

Warning sign electrical area

The following picture shows the warning sign on the electrical section cover:

Meaning of the warning signs

The following table explains the meaning of the warning signs:

Warning sign

Meaning

 

Warning: hot surfaces

 

 

 

Electric current hazard

 

 

Note

You are obliged to keep the warning signs on the instrument complete and in a legible condition.

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Warning: changes to the instrument

Safe instrument

The analyzer is designed and delivered in such a way to ensure safe working if you observe the instructions in the operating instructions.

Warning: Changes to the instrument

If you make any changes to the instrument, you risk rendering the instrument unsafe.

The consequences would be:

Injuries to the operating personnel

Damages to the instrument

loss of warranty.

Therefore, never make any unauthorized additions/conversions to the instrument.

Warning: unsuitable spare parts and consumables

Warning

If you use spare parts and consumables of an unsuitable type and quality, you risk:

Injuries to the operating personnel

damage to the instrument

Distortion of analysis results

Loss of warranty.

Only use original spare parts and original consumables that you have purchased from BÜCHI Labortechnik AG or authorized dealers.

Required user knowledge and skills

Knowledge and skills

Depending on the specific task, the user must have different knowledge and skills. The following table indicates which sections of the operating instructions require what knowledge and skills:

Section

Required knowledge and skills

Work performed by the system

Personnel with good knowledge of the operating system

administrator

and administrative settings.

 

 

Starting up or shutting down the

Personnel authorized by BÜCHI and having undergone

instrument

training.

Using the instrument

Personnel with basic knowledge of chemistry and

 

experience with laboratory work (e.g. laboratory worker).

 

 

Maintaining the instrument

Personnel authorized by BÜCHI.

 

 

Repairing the instrument

Personnel authorized by BÜCHI and having undergone

 

training.

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Required personal safety equipment

Protective glasses

You require protective glasses for many activities. Make sure that protective glasses are always available nearby the analyzer.

Protective gloves

BÜCHI two kinds of protective gloves with the instrument:

The protective leather gloves for protection against cuts on broken glass from cold quartz components.

The heat protection gloves for protection against burns on hot components.

Always keep the protective gloves nearby the analyzer. Replace the protective gloves immediately if required.

Laboratory clothing

For work on and with the instrument you need:

Sturdy shoes

Cotton apron

Hair tie to tie back long hair

Obedience of general rules for safe work in the laboratory

Warning notes during operation

Note

Always pay attention to careful handling when working with the instrument, especially for modifications, maintenance and repairing works. The following notes have to be strictly observed when performing the corresponding works.

Replacing the ash crucible/finger

Please observe the following instructions:

Warning Hot instrument parts and hot ash particles!

Risk of burning due to hot instrument parts.

When replacing:

Wear protective glasses.

Wear the enclosed heat protection gloves.

Place the hot instrument tubes in a tube rack on a level, non-combustible surface.

Protect the hot instrument parts from unauthorized access.

Never leave the instrument unattended when the furnace has been pulled out.

Warning Gas pressure and caustic substances in the instrument

Consumables may escape under pressure and cause chemical burns. Before performing the work:

Shut off the gas supply. To do so, execute the Options > Maintenance > Replace parts command.

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Damaged base panel

Please observe the following instruction:

Caution Damaged base panel!

Damage to the base panel will impair proper functioning of the carousel.

Before starting maintenance work, always remove all samples from the carousel. When dismantling and cleaning the carousel:

Never use pointed objects to dismantle the carousel.

Never use sharp or aggressive cleaners.

Gas pressure

Please observe the following instruction:

Warning Gas pressure and caustic substances in the instrument

Consumables may escape under pressure and cause chemical burns. Before performing the work:

Shut off the gas supply. To do so, execute the Options > Maintenance > Replace parts command.

Hot instrument parts

Please observe the following instruction:

Warning Hot instrument parts!

Risk of burning due to hot instrument parts. Before performing the work:

Allow the furnaces to cool down

Disconnect the power supply plug

Changing mode

Please observe the following instruction:

Caution Overheating if tube fillings are not appropriate for the operating mode! Overheated tube fillings melt, run into the furnace area and destroy the furnace. Make sure that the tube fillings correspond to the selected operating mode.

Cleaning and installing/removing the quartz glass bridge

Please observe the following instruction:

Warning Sharp pieces of broken glass!

When cold quartz or glass components break there is a risk of cut injuries.

Wear the enclosed protective leather gloves and protective glasses when handling cold quartz and glass parts.

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Removing reaction tubes

Please observe the following instructions:

Warning Hot reaction tubes!

Risk of burning due to hot instrument parts.

When replacing the reaction tubes:

Wear protective glasses.

Wear the enclosed heat protection gloves.

Place the hot tubes in a tube rack on a level, non-combustible surface.

Protect the hot tubes from unauthorized access.

Never leave the instrument unattended when the furnace has been pulled out.

Warning Gas pressure and caustic substances in the instrument

Consumables may escape under pressure and cause chemical burns. Before performing the work:

Shut off the gas supply. To do so, execute the Options > Maintenance > Replace parts command.

Filling reaction tubes

Please observe the following instructions:

Warning Sharp pieces of broken glass!

When cold quartz or glass components break there is a risk of cut injuries.

Wear the enclosed protective leather gloves and protective glasses when handling cold quartz and glass parts.

Caution Cutting sealing elements apart/out (o-rings, quad rings, half shells, ferrules).

When cutting sealing elements apart/out with a knife you may damage sealing surfaces.

Never remove sealing elements with a knife but rather with tweezers.

Installing and conditioning the reaction tubes

Please observe the following instructions:

Warning Hot components in the instrument

When working inside the instrument there is a risk of burning as many parts of the instrument are hot.

When working inside the instrument always wear protective glasses and the enclosed heat protection gloves.

Caution Overheating if tube fillings are not appropriate for the operating mode! Overheated tube fillings melt, run into the furnace area and destroy the furnace. Make sure that the tube fillings correspond to the selected operating mode.

Emptying reaction tubes

Please observe the following instruction:

Warning Sharp pieces of broken glass!

When cold quartz or glass components break there is a risk of cut injuries.

Wear the enclosed protective leather gloves and protective glasses when handling cold quartz and glass parts.

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Warning Harmful substances when glass is broken!

When filled quartz or glass components break there is a risk that harmful substances may be released.

Wear a dust mask when handling cold quartz and glass parts.

Replacing fuses

Please observe the following instructions:

Risk

Live parts!

 

When replacing fuses there is a risk of electrocution.

 

Before replacing fuses:

 

Allow the furnaces to cool down.

 

Disconnect the power supply plug.

 

 

Risk

High voltage!

 

Using the wrong fuses can pose a risk of electrocution or fire.

 

Only use fuses matching the indicated type and the indicated voltage on the fuse

 

holder.

 

 

Caution

Lack of ventilation of the analyzer!

 

A lack of ventilation leads to overheating of the analyzer. Before you switch off the

 

instrument:

 

Ste the setpoint temperatures of the furnaces to 0 °C. To do so execute the

 

command Options > Settings > Parameter > Temperatures

 

Allow the furnaces to cool down until the temperature displayed is less than

 

55 °C

Filling the drying tube

Please observe the following instructions:

Warning Caustic substance Sicapent® (phosphorus pentoxide)!

Danger of chemical burns when handling Sicapent®.

Wear protective glasses and the enclosed protective leather gloves.

Warning Sharp pieces of broken glass!

When cold quartz or glass components break there is a risk of cut injuries.

Wear the enclosed protective leather gloves and protective glasses when handling cold quartz and glass parts.

Installing/removing the drying tube

Please observe the following instructions:

Caution Lack of ventilation of the analyzer!

A lack of ventilation leads to component overheating

Do not open the front door too long when the furnaces are hot and the furnace is not pulled out. Otherwise the ventilation will not work properly.

Warning Caustic substance Sicapent® (phosphorus pentoxide)!

Danger of chemical burns when handling Sicapent®.

Wear protective glasses and the enclosed protective leather gloves.

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Overheating of tube fillings

Please observe the following instruction:

Caution Overheating if tube fillings are not appropriate for the operating mode! Overheated tube fillings melt, run into the furnace area and destroy the furnace. Make sure that the tube fillings correspond to the selected operating mode.

Working with the database

Please observe the following instructions:

Caution

Data loss

 

After reorganizing the database via Clean all sample data and the contents of the

 

logbook are irrevocably deleted.

 

Always backup your data before reorganizing the database via Clean.

 

 

Caution

Data loss

 

Restoring the database via Restore irrevocably overwrites all sample data, the

 

contents of the logbook and the database configfuration parameters.

 

Always backup your data before restoring the database via Restore.

 

 

Improper changes

Please observe the following instruction:

Caution Improper changes impair proper operation of the system and may destroy system components.

Only configure the instrument if you are authorized to do so and observe the operating instructions.

Baking out combustion tube and reduction tube

Please observe the following instructions:

Warning Gas pressure and caustic substances in the instrument

Consumables may escape under pressure and cause chemical burns. Before performing the work:

Shut off the gas supply. To do so, execute the Options > Maintenance > Replace parts command.

Warning Hot components in the instrument

When working inside the instrument there is a risk of burning as many parts of the instrument are hot.

When working inside the instrument always wear protective glasses and the enclosed heat protection gloves.

Mixing up gas inlets

Please observe the following instruction:

Caution A mix-up of the gas inlets may lead to destruction of the instrument.

Connect the supply lines carefully and observe the diagram.

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C H A P T E R 3

 

Product description

 

Target group

 

Personnel working with the instrument.

 

Purpose

 

This section provides general information about the instrument.

 

In this chapter

 

Analytical characteristics and technical specifications...................................................................

30

Instrument design..........................................................................................................................

33

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Analytical characteristics and technical specifications

 

Target group

 

Personnel working with the instrument.

 

Purpose

 

This section lists the analytical characteristics and technical specifications.

 

In this section

 

Analytical characteristics ...............................................................................................................

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Technical specifications.................................................................................................................

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