KjelMaster K-375 with KjelSampler K-376/K-377
Operation Manual
11593514 en
Document History
Index Date Author Changes
A 25/MAY/2012 NAGG Initial version
B 16/JUL/2013 NAGG First revised version
Table of contents
Table of contents
1 About this manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .9
1.1 Trademarks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
1.2 Abbreviations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
2 Safety. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
2.1 User qualification . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
2.2 Proper use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
2.3 Improper use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
2.4 Safety warnings and safety signs used in this manual . . . . . . . . . . . . . . . . . 12
2.5 Product safety. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
2.5.1 General hazards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
2.5.2 Instrument-related hazards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
2.5.3 Other hazards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
2.5.4 Personal protective equipment . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
2.5.5 Built-in safety elements and measures. . . . . . . . . . . . . . . . . . . . . . . . . 17
2.6 General safety rules . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
3 Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
3.1 Scope of delivery . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
3.1.1 Basic devices . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
3.1.2 Standard accessories for K-375 . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
3.1.3 Standard accessories for K-376 . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
3.1.4 Standard accessories for K-377 . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
3.1.5 Optional accessories K-375 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
3.1.6 Optional accessories K-376/K-377 . . . . . . . . . . . . . . . . . . . . . . . . . . 25
3.2 Technical data overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
3.2.1 Technical data KjelMaster K-375 and KjelSampler K-376/K-377. . . . . . . . . . . . 26
3.2.2 Technical data titrator . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
3.3 Titration solution. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
3.4 Information on type plate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
3.5 Reference substances. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
3.6 Materials used. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
3.6.1 Titrator module and dosing unit . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
3.6.2 K-375 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
3.6.3 K-376/K-377 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30
Read this manual carefully before installing and running your system and note the safety precautions
in chapter 2 in particular. Store the manual in the immediate vicinity of the instrument, so that it can
be consulted at any time.
No technical modifications may be made to the device without the prior written agreement of BUCHI.
Unauthorized modifications may affect the system safety or result in accidents.
This manual is copyright. Information from it may not be reproduced, distributed, or used for competitive purposes, nor made available to third parties. The manufacture of any component with the aid of
this manual without prior written agreement is also prohibited.
If you need another language version of this manual, you can download it at
www.buchi.com.
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K-375/376/377 Operation Manual, Version B
Table of contents
4 Description of function . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
4.1 Device overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
4.1.1 Opening the service door . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32
4.2 Functional principle of Sampler System K-375 with K-376 or K-377. . . . . . . . . . 33
4.3 Standby function . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
4.4 System preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
4.4.1 Preheating. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
4.4.2 Priming . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
4.4.3 Cleaning. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
4.4.4 Aspiration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
4.5 Distillation and titration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36
4.5.1 Distillation Mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36
4.5.2 Titration Type . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36
4.5.3 Sensor Type . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36
4.5.4 Titration Mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36
4.5.5 Measuring Mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
4.5.6 Titration Algorithm . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
4.5.7 Determination Mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
4.6 Different methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38
4.7 Blank values. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
4.7.1 Blanks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
4.7.2 Control blanks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
4.8 Reference substances. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
4.9 Result Groups . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
4.10 Explanation of alkaline direct distillation . . . . . . . . . . . . . . . . . . . . . . . . 40
5 Putting into operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43
5.1 Installation site. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43
5.2 Electrical connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
5.2.1 Connections of the K-375 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
5.2.2 Connections of the K-376/K-377 . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
5.3 Transfer connection K-376 (K-377) – K-375 . . . . . . . . . . . . . . . . . . . . . . 46
5.3.1 Connecting the K-376 to the K-375 . . . . . . . . . . . . . . . . . . . . . . . . . . 46
5.3.2 Connecting the transfer hoses of the K-377 . . . . . . . . . . . . . . . . . . . . . . 48
5.4 Reagent/water and waste connections . . . . . . . . . . . . . . . . . . . . . . . . 49
5.5 Buret unit for titrant . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51
5.6 Storage tank connection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52
5.7 Level sensors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 53
5.8 Connections to peripheral devices. . . . . . . . . . . . . . . . . . . . . . . . . . . 55
5.8.1 Connecting a printer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55
5.8.2 Connecting a network cable . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55
5.8.3 Connecting a KjelSampler K-376 or K-377 . . . . . . . . . . . . . . . . . . . . . . 55
5.8.4 Connecting a balance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55
5.8.5 Connecting a bar code reader . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 56
5.8.6 External dosing unit for back titration . . . . . . . . . . . . . . . . . . . . . . . . . 56
5.8.7 Electrode connection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 56
5.9 Preparing the system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57
5.9.1 Preparing the software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57
5.9.2 Preparing the hardware . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 58
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K-375/376/377 Operation Manual, Version B
Table of contents
6 Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
6.1 The operating principle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
6.2 The home screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
6.2.1 The title bar . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61
6.2.2 The bottom bar . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61
6.2.3 System status icons . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62
6.3 User concept . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 63
6.4 Editable and non-editable menu items. . . . . . . . . . . . . . . . . . . . . . . . . 63
6.5 The status view . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65
6.5.1 RESULT display . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 67
6.5.2 CHART display . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 67
6.5.3 INFO display . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 68
6.6 Determination . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69
6.6.1 System Preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 70
6.6.2 Single Sample . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 77
6.6.3 Sample Lists. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 79
6.6.4 Sequences . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 83
6.7 Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 89
6.7.1 Result groups . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 89
6.7.2 Last Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 92
6.7.3 Blank Correction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 93
6.8 Determination Parameters. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97
6.8.1 Methods. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97
6.8.2 Volumetric Solutions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .106
6.8.3 Reference Substances . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .107
6.9 Device. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .108
6.9.1 Settings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .108
6.9.2 Utilities. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .115
6.9.3 Diagnostics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .117
6.9.4 Logout . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .117
7 Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .119
7.1 Daily maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .120
7.1.1 Before sample determination . . . . . . . . . . . . . . . . . . . . . . . . . . . . .120
7.1.2 After sample determination . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .121
7.1.3 pH electrode/pH calibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .121
7.1.4 Filling boric acid into receiving vessel after last sample of rack was determined . . . .122
7.2 Weekly maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .123
7.2.1 Cleaning the housing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .123
7.2.2 Cleaning the titrator . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .123
7.2.3 Cleaning the glass parts of the dosing unit . . . . . . . . . . . . . . . . . . . . . .123
7.2.4 Cleaning the dip tube of the sampler . . . . . . . . . . . . . . . . . . . . . . . . .123
7.2.5 Device monitoring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .124
7.3 Monthly maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .125
7.3.1 Calibrating the pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .125
7.3.2 Checking the distillate amount . . . . . . . . . . . . . . . . . . . . . . . . . . . . .126
7.3.3 Inspecting the buret . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .127
7.3.4 Inspecting the titrator . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .127
7.3.5 Inspecting the sample tubes. . . . . . . . . . . . . . . . . . . . . . . . . . . . . .127
7.4 Half-yearly maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .128
7.4.1 K-375 Sealing between sample tube and splash protector . . . . . . . . . . . . . .128
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K-375/376/377 Operation Manual, Version B
Table of contents
7.4.2 K-376/K-377 dip tube and sealing cap . . . . . . . . . . . . . . . . . . . . . . . .129
7.4.3 Replacing the splash protector . . . . . . . . . . . . . . . . . . . . . . . . . . . .131
7.5 Yearly maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .133
7.5.1 Replacement of wear parts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .133
7.5.2 Decalcification of the steam generator . . . . . . . . . . . . . . . . . . . . . . . . .134
7.5.3 Replacement of the sodium hydroxide pump . . . . . . . . . . . . . . . . . . . . .134
7.5.4 Replacement of the wave spring. . . . . . . . . . . . . . . . . . . . . . . . . . . .136
7.6 Replace every two years . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .137
7.6.1 Replacement of the transfer connection . . . . . . . . . . . . . . . . . . . . . . . .137
7.7 Maintenance work if required . . . . . . . . . . . . . . . . . . . . . . . . . . . . .138
7.7.1 Changing the buret tip. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .138
7.7.2 Cleaning the pH electrode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .139
7.7.3 Replacing the buret . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .139
7.7.4 Cleaning the splash protector and the rubber seal . . . . . . . . . . . . . . . . . . .139
7.7.5 Glass parts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .140
7.7.6 Troubleshooting the dosing unit . . . . . . . . . . . . . . . . . . . . . . . . . . . .140
7.7.7 Adjusting the sample tube holder . . . . . . . . . . . . . . . . . . . . . . . . . . .140
7.8 Customer service . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .142
8 Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .143
8.1 Problems that may occur . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .143
8.2 Error messages on the display of the K-375. . . . . . . . . . . . . . . . . . . . . .146
8.3 Eliminating errors of the KjelSampler K-376/K-377 . . . . . . . . . . . . . . . . . .150
8.4 Eliminating errors of the titrator . . . . . . . . . . . . . . . . . . . . . . . . . . . .151
9 Taking out of operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .153
9.1 Emptying the steam generator . . . . . . . . . . . . . . . . . . . . . . . . . . . .153
9.2 Emptying the buret of the titrator . . . . . . . . . . . . . . . . . . . . . . . . . . .154
9.3 Storage/shipping . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .154
9.4 Disposal. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .154
10 Spare parts. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .155
10.1 Spare parts K-375 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .155
10.2 Spare parts K-376/K-377 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .156
10.3 Hosing connection scheme Kjeldahl Sampler System K-375/K-376. . . . . . . . . .156
11 Declarations and requirements. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .157
11.1 FCC requirements (for USA and Canada) . . . . . . . . . . . . . . . . . . . . . . .157
11.2 Declaration of conformity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .158
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K-375/376/377 Operation Manual, Version B
1 About this manual
This manual describes the KjelMaster Sampler System K-375/K-376/K-377 and provides all information required for its safe operation and to maintain it in good working order.
It is addressed to laboratory personnel in particular.
NOTE
The symbols pertaining to safety (DANGER, CAUTION and WARNING) are explained in chapter 2.
1.1 Trademarks
DURAN® is a registered trademark of the SCHOTT AG.
1.2 Abbreviations
CSM: Chopped Strand Mat
ETFE: Polytetrafluorethylene
FEP: Fluorinated Ethylene Propylene
KCI: Potassium chloride
PCTFE: Polychlorotrifluoroethylene
PMMA: Polymethyl methacrylate
POM: Polyoxymethylene
PP: Polypropylene
PTFE: Ethylenetetrafluoroethylene
PUR: Polyurethane
UV: Ultraviolet
EPDM: Ethylene propylene diene monomer
PVDF: polyvinylidene difluoride
PA: Polyamide
1 About this manual
9
K-375/376/377 Operation Manual, Version B
1 About this manual
10
K-375/376/377 Operation Manual, Version B
2 Safety
This chapter points out the safety concept of the device and contains general rules of behavior and
warnings from hazards concerning the use of the product.
The safety of users and personnel can only be ensured if these safety instructions and the safety
related warnings in the individual chapters are strictly observed and followed. Therefore, the manual
must always be available to all persons performing the tasks described herein.
2.1 User qualification
The device may only be used by laboratory personnel and other persons who on account of training
or professional experience have an overview of the dangers which can develop when
operating the instrument.
Personnel without this training or persons who are currently being trained require careful instruction.
The present Operation Manual serves as the basis for this.
2 Safety
2.2 Proper use
The device has been designed and built for laboratories. It serves for nitrogen determination
according to Kjeldahl. The KjelMaster K-375 as stand-alone device may also be used for distillations
of steam-volatile substances.
2.3 Improper use
Applications not mentioned above are improper. Also applications which do not comply with the
technical data are considered improper.
The operator bears the sole risk for any damages caused by such improper use.
The following uses are expressly forbidden:
• Use of the device in rooms which require ex-protected devices.
• Use on samples which can explode or inflame (e.g.: explosives, etc.) due to shock, friction, heat or
spark formation.
!
Danger
During any improper use, the effectiveness of the protection systems of the devices
can be affected.
• Avoid any improper use of the devices!
11
K-375/376/377 Operation Manual, Version B
2.4 Safety warnings and safety signs used in this manual
DANGER, WARNING, CAUTION and NOTICE are standardized signal words for identifying levels of
hazard seriousness of risks related to personal injury and property damage. All signal words, which
are related to personal injury are accompanied by the general safety sign.
For your safety it is important to read and fully understand the table below with the different signal
words and their definitions!
Sign Signal word Definition Risk level
DANGER
Indicates a hazardous situation which, if not avoided, will result in
death or serious injury.
2 Safety
★★★★
WARNING
CAUTION
NOTICE
no
Supplementary safety information symbols may be placed in a rectangular panel on the left to the
signal word and the supplementary text (see example below).
Space for
supplementary
safety
information
symbols.
Table of supplementary safety information symbols
The reference list below incorporates all safety information symbols used in this manual and their
meaning.
Symbol Meaning
Indicates a hazardous situation which, if not avoided, could result
in death or serious injury.
Indicates a hazardous situation which, if not avoided, may result
in minor or moderate injury.
Indicates possible property damage, but no
practices related to personal injury.
SIGNAL WORD
Supplementary text, describing the kind and level of hazard / risk seriousness.
• List of measures to avoid the herein described, hazard or hazardous situation.
• ...
• ...
(property damage only)
★★★☆
★★☆☆
★☆☆☆
12
General warning
Electrical hazard
Biohazard
Hot surface
K-375/376/377 Operation Manual, Version B
Symbol Meaning
Heavy weight, avoid overexertion
Chemical burns by corrosives
Pinch point. Mechanical hazard.
Fragile components
2 Safety
Explosive gases, explosive environment
Device damage
Wear laboratory coat
Wear protective goggles
Wear protective gloves
Additional user information
Paragraphs starting with NOTE transport helpful information for working with the device / software or
its supplementaries. NOTEs are not related to any kind of hazard or damage (see following example).
NOTE
Useful tips for the easy operation of the instrument / software.
13
K-375/376/377 Operation Manual, Version B
2.5 Product safety
The device is designed and built in accordance with current state-of-the-art technology. Nevertheless, risks to users, property, and the environment can arise when the device is used carelessly or
improperly.
The manufacturer has determined residual dangers emanating from the instrument
• if the device is operated by insufficiently trained personnel.
• if the device is not operated according to its proper use.
Appropriate warnings in this manual serve to make the user alert to these residual dangers.
2.5.1 General hazards
The following safety messages show hazards of general kind which may occur when handling the
instrument. The user shall observe all listed counter measures in order to achieve and maintain the
lowest possible level of hazard.
Additional warning messages can be found whenever actions and situations described in this manual
are related to situational hazards.
2 Safety
!
Death or serious injuries by use in explosive environments.
• Do not store or operate the device in explosive environments.
• Remove all sources of flammable vapors.
• Do not store chemicals in the vicinity of the device.
!
Risk of minor or moderate cuts by sharp edges.
• Do not touch defective or broken glassware with bare hands.
• Do not touch thin metal edges.
Risk of device damage by liquids or mechanical shocks.
• Do not spill liquids over the device or its components.
• Do not drop the device or its components.
• Keep external vibrations away from the instrument.
2.5.2 Instrument-related hazards
DANGER
CAUTION
NOTICE
14
!
CAUTION
Risk of injury.
• Never touch the surface of the touchscreen with pointed or sharp objects! Otherwise the
screen might get damaged and splinter.
K-375/376/377 Operation Manual, Version B
2 Safety
!
CAUTION
Risk of burns by hot surface. Surface temperature exceeds 60 °C.
• Do not touch hot surfaces of the instrument.
!
CAUTION
Risk of pinch point injuries.
• In order to avoid injuries to the hands and fingers the K-376 and K-377 KjelSamplers may not
be manipulated during the moving action of the sampler arm.
!
CAUTION
Risk of burns by hot steam.
• The system works with hot steam. Avoid any contact with hot steam.
!
DANGER
Risk of chemical burns by corrosives.
• Wear laboratory coat, protective gloves and protective goggles at all times.
!
DANGER
Risk of chemical burns by corrosives.
• During operation the sample tube contains either strong acid or strong base. In case the
sample tube brakes, the content of the sample tube is collected in the drip tray on the bottom
of the housing. Wear laboratory coat protective gloves and protective goggles when emptying
the drip tray.
15
K-375/376/377 Operation Manual, Version B
2.5.3 Other hazards
Fundamental dangers arise from.
• acids and lye
• flammable gases or solvent fumes in the direct vicinity of the instrument
• damaged glass parts
• insufficient distance between the device and the wall (see chapter 5.1, Installation site)
• burns caused by contact with hot glass parts
• burns caused by contact with steam at the waste-outlet
• defective transfer tube: escape of steam and/or sulfuric acid
2.5.4 Personal protective equipment
Always wear personal protective equipment such as protective eye goggles, protective clothing
and gloves. The personal protective equipment must meet all requirements of all data sheets for
the chemicals used. These instructions are an important part of the K-375, K-376 and K-377 and
must be made available at all times to the operating personnel at the place where the equipment is
deployed. This also applies to additional language versions of these instructions, which can be reordered separately.
2 Safety
!
WARNING
Serious chemical burns by corrosives.
• Observe all data sheets of the used chemicals.
• Handle corrosives in well ventilated environments only.
• Always wear protective goggles.
• Always wear protective gloves.
• Always wear protective clothes.
• Do not use damaged glassware.
16
K-375/376/377 Operation Manual, Version B
2.5.5 Built-in safety elements and measures
The KjelMaster K-375 has monitored protective doors which prevent a distillation to start while a
door is open. A running distillation is immediately interrupted when a door is opened. The dosing of
reagents is also immediately stopped.
The sample changers K-376/K-377 have monitored protective shields. Running a sample changer
with opened shield is impossible. For the K-377 only the shield of the tray, that is currently not in use
can be opened.
K-375:
• Protective door: Safety appliance to protect users from burns at the splash protector (distillation
area) which is hot during distillation.
• Protective door sensors: Prevents to start a distillation with the protective doors open and stops
the distillation as soon as a protective door is opened during the process.
• Sample tube sensor: Prevents to start a distillation without a sample tube inserted.
• Service door sensor/switch: Electrical power is disconnected immediately when the service door
is opened, thus preventing electrical shock during maintenance.
K-376:
• Protective shield with sensor/switch: As soon as the shield is opened an alarm sound is triggered
and any movement of the arm is stopped.
2 Safety
K-377:
• Protective shield with sensor/switch: As soon as the shield of the tray in use is opened an alarms
sound is triggered and any movement of the arm is stopped. (The shield of the respective tray
that is not operated can still be opened without any restrictions.)
2.6 General safety rules
Responsibility of the operator
The head of the laboratory is responsible for training his/her personnel.
The operator shall inform the manufacturer without delay of any safety-related incidents which might
occur during operation of the device or its accessories. Legal regulations, such as local, state and
federal laws applying to the device or its accessories must be strictly followed.
Duty of maintenance and care
The operator is responsible for the proper condition of instrument. This includes maintenance, service
and repair jobs that are performed on schedule by authorized personnel only.
Spare parts to be used
Use only genuine consumables and spare parts for maintenance to assure good system performance, reliability and safety. Any modifications of spare parts or assemblies are only allowed with the
prior written permission of the manufacturer.
Modifications
Modifications to the device are only permitted after prior consultation and with the written approval
of the manufacturer. Modifications and upgrades shall only be carried out by an authorized BUCHI
technical engineer. The manufacturer will decline any claim resulting from unauthorized modifications.
17
K-375/376/377 Operation Manual, Version B
2 Safety
18
K-375/376/377 Operation Manual, Version B
3 Technical data
This chapter introduces the reader to the device specifications. It contains the scope of delivery,
technical data, requirements and performance data.
3.1 Scope of delivery
3.1.1 Basic devices
3 Technical data
Table 3-1: KjelMaster K-375
Product Order number
KjelMaster K-375
with glass splash protector and
potentiometric sensor
(220 – 240 V, 50/60 Hz)
KjelMaster K-375
with glass splash protector and
colorimetric sensor
(220 – 240 V, 50/60 Hz)
KjelMaster K-375
with plastic splash protector and
potentiometric sensor
(220 – 240 V, 50/60 Hz)
KjelMaster K-375
with plastic splash protector and
colorimetric sensor
(220 – 240 V, 50/60 Hz)
Table 3-2: KjelSampler K-376
Product Order number
KjelSampler K-376
with one tray
(100 – 240 V, 50/60 Hz)
113751700
113752700
113753700
113754700
113750710
19
Table 3-3: KjelSampler K-377
Product Order number
KjelSampler K-377
with two trays
(100 – 240 V, 50/60 Hz)
K-375/376/377 Operation Manual, Version B
113750720
3 Technical data
Table 3-4: KjelMaster/Sampler Systems
K-375/K-376
Product Order number
KjelMaster Sampler System K-375/K-376
113751710
K-375 with glass splash protector and
potentiometric sensor
K-375: 220 – 240 V, 50/60 Hz
K-376/K-377: 100 – 240 V, 50/60 Hz
KjelMaster Sampler System K-375/K-376
113752710
K-375 with glass splash protector and
colorimetric sensor
K-375: 220 – 240 V, 50/60 Hz
K-376/K-377: 100 – 240 V, 50/60 Hz
KjelMaster Sampler System K-375/K-376
113753710
K-375 with plastic splash protector and
potentiometric sensor
K-375: 220 – 240 V, 50/60 Hz
K-376/K-377: 100 – 240 V, 50/60 Hz
KjelMaster Sampler System K-375/K-376
113754710
K-375 with plastic splash protector and
colorimetric sensor
K-375: 220 – 240 V, 50/60 Hz
K-376/K-377: 100 – 240 V, 50/60 Hz
Table 3-5: KjelMaster/Sampler Systems
K-375/K-377
Product Order number
KjelMaster Sampler System K-375/K-377
K-375 with glass splash protector and
potentiometric sensor
K-375: 220 – 240 V, 50/60 Hz
K-376/K-377: 100 – 240 V, 50/60 Hz
KjelMaster Sampler System K-375/K-377
K-375 with glass splash protector and
colorimetric sensor
K-375: 220 – 240 V, 50/60 Hz
K-376/K-377: 100 – 240 V, 50/60 Hz
KjelMaster Sampler System K-375/K-377
K-375 with plastic splash protector and
potentiometric sensor
K-375: 220 – 240 V, 50/60 Hz
K-376/K-377: 100 – 240 V, 50/60 Hz
KjelMaster Sampler System K-375/K-377
K-375 with plastic splash protector and
colorimetric sensor
K-375: 220 – 240 V, 50/60 Hz
K-376/K-377: 100 – 240 V, 50/60 Hz
113751720
113752720
113753720
113754720
20
K-375/376/377 Operation Manual, Version B
3.1.2 Standard accessories for K-375
11057410
43178
43185
43407
49151
3 Technical data
Table 3-6: Standard accessories for K-375
Number
of pieces
Product Order number
1 Pair of glass tongs 02004
1 Connection cable RJ45 length
44989
2 m
1 Mains cable of the following
types
Type CH 10010
Type Schuko/Japan 10016
Type GB 17835
Type AUS 17836
Type USA 33763
1 pH electrode
or (according to purchase order)
colorimetric sensor
1 Indicator according to Sher,
11056842
11057410*
003512
100 mL
(if device version with colorimetric sensor is shipped)
1 Buffer set pH 4 and pH 7
43188
(3 x 20 mL each)
1 KCI electrolyte, sat. , 250 mL 11059759
43457
11058157
11055914
11056835
11056836
1 Hose connector in line 11–13 43178*
1 Hose chemical supply, Nyflex,
43185*
length 6 m, Ø 5/10 mm
3 Suction tube to tanks, FEP,
43407*
length 580 mm
1 Connection grommet 49151*
2 Hose waste drain, EPDM,
43457*
L = 1.8 m, ø 11/18 mm
5 Clamp D15.6 49167
1 Silicone hose ø 8 mm/12x1.8m 11058157*
1 Clamp D12.8 43297
1 Y-piece ø12 mm 11058358
1 Cooling water hose complete:
37780
G 3/4”, G 1/2”, L = 1.5 m
3 Clamp D11.9 43841
2 O-ring 190.1 x 3.53 EPDM 75 49676
2 O-ring 247.2 x 3.53 EPDM 11058241
4 Level sensor 11055914*
1 Laboratory vessel 53203
1 Dosino 800 11056835*
1 Dosing unit 11056836*
21
K-375/376/377 Operation Manual, Version B
3 Technical data
43203
11058252
Table 3-6: Standard accessories for K-375
(continued)
11059802
11057779
3.1.3 Standard accessories for K-376
43482
11057711
Number
of pieces
Product Order number
1 Gauge sample tube holder 11059802
2 Tank 10 L, without caps 43410
2 Cap for 10 L tank, large 25869
4 Cap for 10 L and 20 L tank, small 43477
4 Tank labels 43434
2 Tank 20 l, without caps 43408
2 Cap for 20 L tank, large 43478
1 Distance holder buret tip 43203*
1 Mini gender changer 43108
1 Weighing boat 40444
4 EPDM sealing for tanks 43048
1 Open end spanner 11058252*
1 Tool SVL 22 11057779*
Table 3-7: Standard accessories for K-376
Number of
pieces
1 K-376/K-377 cable RS232
Product Order number
43920
(crossed)
1 Sample tube 300 mL 3904
1 Sample tube 500 mL 26128
1 Clamp ring 43238
1 Hose clamp 22352
1 Fastener for transfer tube 43482*
6 Sample tubes (set of 4), 300 mL 37377
1 Express rack, 4 places 11057711*
1 Rack complete, 20 places 11059831*
22
11059831
11058240
1 Mains cable of the following
types
Type CH 10010
Type Schuko/Japan 10016
Type GB 17835
Type AUS 17836
Type USA 33763
1 Test gauge for sample tubes 11058240
K-375/376/377 Operation Manual, Version B
3.1.4 Standard accessories for K-377
11058240
3 Technical data
Table 3-8: Standard accessories for K-377
Number of
pieces
1 K-376/K-377 cable RS232
Product Order
number
43920
(crossed)
2 Sample tube 300 mL 3904
1 Sample tube 500 mL 26128
1 Clamp ring 43238
1 Hose clamp 22352
1 Fastener for transfer tube 43482
12 Sample tubes (set of 4), 300 mL 37377
2 Rack complete, 20 places 38621
1 Mains cable of the following types
Type CH 10010
Type Schuko/Japan 10016
Type GB 17835
Type AUS 17836
Type USA 33763
1 Test gauge for sample tubes 11058240
Table 3-9: Operation Manuals and Quick Guides
Product Order number
Operation Manual:
English 11593514
German 11593515
French 11593516
Italian 11593517
Spanish 11593518
Chinese 11593519
Japanese 11593520
23
K-375/376/377 Operation Manual, Version B
3.1.5 Optional accessories K-375
43333
43390
3 Technical data
Table 3-12: Optional accessories K-375
Product Order number
Sample tubes (set of 4), 300 mL 37377
Sample tube 500 mL 26128
Sample tubes (set of 4), 500 mL 43982
Pair of glass tongs 02004
Receiving vessel 340 mL 43333*
Receiving vessel 420 mL 43390*
Devarda splash protector 43335
Tanks without level sensors, including caps
10 L chemicals 43468
10 L waste 43470
20 L chemicals 43469
20 L waste 43471
11056851
Level sensor 11055914
O-ring level sensor (10 L tank) 49676
O-ring level sensor (20 L tank) 11058241
Spectrosense 610 nm with cable 11057410
Buffer solution pH 4, 1000 mL 26321
Buffer solution pH 7, 1000 mL 26322
Indicator according to Sher, 100 mL 03512
Temperature sensor for titrator 11056851*
Dosing unit (for back titration) 11056836
Motor for dosing unit 11056835
Sample tube holder for 4 sample tubes,
16951
500 mL each
IQ/OQ Package K-375 (English) 11058677
IQ/OQ Package K-375/K-376/K-377
11058678
(English)
Repeating OQ Package K-375 (English) 11058679
Repeating OQ Package K-375/K-
11058680
376/K-377 (English)
24
K-375/376/377 Operation Manual, Version B
3.1.6 Optional accessories K-376/K-377
3 Technical data
Table 3-14: Optional accessories for K-376/K-377
Product Order number
Stand for rack 11058659
Sample tubes (set of 4), 500 mL 43982
Rack for 12 sample tubes, 500 mL 43970*
Retainer plate (holds tubes firmly in rack
43970
for machine washing)
Set of 10 boiling rods for digestion of
samples with tendency of boiling retardation (alternative for boiling chips)
Sample tubes (set of 4), 300 mL 37377
Dip tube with cross-slot for soil/stone
containing samples
Glassfinger for sample tubes
for soil samples
38559
43087
47845
48638
25
K-375/376/377 Operation Manual, Version B
3.2 Technical data overview
3.2.1 Technical data KjelMaster K-375 and KjelSampler K-376/K-377
Table 3-15: Technical data
KjelMaster K-375 KjelSampler K-376 KjelSampler K-377
Connection voltage 220 – 240 VAC ±10% 100 – 240 VAC ± 10 % 100 – 240 VAC ± 10 %
Frequency 50/60 Hz 50/60 Hz 50/60 Hz
Power consumption max. 2.2 kW max. 150 W max. 150 W
Current consumption (230 V) 9.5 A 650 mA 650 mA
Weight 32 kg 40 kg
3 Technical data
64 kg
(without rack and sample
tubes)
Dimensions (W x H x D) 458 x 670 x 431 mm 505 x 750* x 655
* 1000 mm height
required to allow free
movement of the sampler
arm
(without rack and sample
tubes)
1015 x 750** x 655
**1250 mm height
required to allow free
movement of the sampler
arm
Interfaces RS232 RS232 RS232
Recovery rate > 99.5 % (1 – 200 mg N)
Reproducibility (RSD) < 1 %
Measuring range 0.1 – 200 mg N
Environmental conditions
Temperature
Altitude
Humidity
for indoor use only
+ 5 °C to + 40 °C
up to 2000 m above sea level
maximum relative humidity 80 % for temperatures up to 31 °C, decreasing linearly to
50 % relative humidity at 40 °C
Mains connection Device plug C14 Device plug C14 Device plug C14
Overvoltage category II II II
Pollution degree 2 2 2
Approval CE/CSA CE/CSA CE/CSA
3.2.2 Technical data titrator
The following sensors can be connected to the titrator:
• combined pH glass electrode
• optical sensor with measuring range between 50 and 1000 mV (max. 1200 mV)
• temperature measuring sensor for Resistance Thermometer Pt 1000, connection: 2 x 4 mm
sockets and 1 x 2 mm socket
Dosing accuracy:
According to DIN EN ISO 8655, Part 3, or better
Typical accuracy: Systematic error max. ± 30 µL
26
K-375/376/377 Operation Manual, Version B
3 Technical data
Measuring input: pH/mV input with 12 bit transducer for accurate resolution during the titration
Connection:
Measuring range Display resolution Accuracy* without sensor Input resistance (Ω)
pH 0…14 0.01 0.05 ±1 digit > 5·10
mV –1400 ... +1400 0.1 2 ±1 digit > 5·10
Measuring range Display resolution Accuracy* without sensor
T [°C] –30…115 0,1 0,5 K ±1 digit
*Accuracy:
Indicated in terms of measuring incertainty with a confidence of 95%. In addition the measuring uncertainty of the sensor has to be taken into account as well. For pH electrodes e.g.: ∆ pH= 0.012...0.03
according to DIN 19 266, Part 3.
3.3 Titration solution
The amount of sample and the concentration of the titrant should be optimized, so that the titrant
volume is between 3 and 17 mL (buret volume: 20 mL).
Table 3-16: Nitrogen expected
N-amount N-content Sample size Titrant Titrant concentration Titrant volume
5 mg N 0.5 % N 1 g
50 mg N 5 % N 1 g
100 mg N 10 % N 1 g
100 mg N 10 % N 1 g
200 mg N 20 % N 1 g
200 mg N 20 % N 1 g
electrode socket according to DIN 19 262 or BNC socket and reference electrode 1 x 4 mm socket
12
12
H2SO4 0.01 mol/L
H2SO4 0.1 mol/L
H2SO4 0.25 mol/L
H2SO4 0.5 mol/L
H2SO4 0.5 mol/L
H2SO4 1 mol/L
17.8 mL
17.8 mL
14.3 mL
7.1 mL
14.3 mL
7.1 mL
Table 3-17: Protein expected
P-content P-factor N-content Sample size Titrant Titrant concentration Titrant volume
1 % P 6.25 0.16 % N 2 g
2 % P 6.25 0.32 % N 1 g
5 % P 6.25 0.80 % N 2 g
10 % P 6.25 1.6 % N 2 g
10 % P 6.25 1.6 % N 2 g
20 % P 6.25 3.2 % N 2 g
50 % P 6.25 8.0 % N 2 g
H2SO4 0.01 mol/L
H2SO4 0.01 mol/L
H2SO4 0.1 mol/L
H2SO4 0.1 mol/L
H2SO4 0.25 mol/L
H2SO4 0.25 mol/L
H2SO4 0.5 mol/L
11.4 mL
11.4 mL
5.7 mL
11.4 mL
4.6 mL
9.1 mL
11.4 mL
General recommendation
The correction factor for self prepared solutions is called titer.
The use of standardized titration solutions make a titer determination unnecessary.
Exact titrant concentration = concentration x titer
The titer of the titrant must be known. In case, it is unknown, it must be determined.
Example: Exact titrant concentration = 0.100 mol/L x 0.998
27
K-375/376/377 Operation Manual, Version B
3.4 Information on type plate
a Device type code
b Serial number
3 Technical data
c Supply voltage range/type
d Frequency of supply voltage
e Nominal power rating
f Year of manufacture
28
K-375/376/377 Operation Manual, Version B
3.5 Reference substances
Table 3-18: Reference substances
Name Purity % N theoretical
Ammonium
99.5 12.18 0.2 g c(H2SO4) = 0.1 mol/L No
dihydrogen
phosphate
Glycine 99.7 18.66 0.2 g c(H
Phenylalanine 99.0 8.47 0.3 g c(H2SO4) = 0.1 mol/L Yes
Ammonium
99.5 21.21 0.2 g c(H2SO4) = 0.1 mol/L No
sulfate
Tryptophan 99.0 13.72 0.2 g c(H
Acetanilide 99.0 10.36 0.2 g c(H2SO4) = 0.1 mol/L Yes
3.6 Materials used
(100 % purity)
Recommended
sample size
3 Technical data
Recommended titrant concentration Digestion necessary
2SO4) = 0.1 mol/L Yes
2SO4) = 0.1 mol/L Ye s
3.6.1 Titrator module and dosing unit
Table 3-19: Materials on the titrator
part Material designation
Housing sheet steel
NOTE
For the materials of the Dosing Unit, please refer to its manual which is delivered together with
dosing unit.
3.6.2 K-375
Table 3-20: Material on the K-375
Part Material Material code
Housing Polyurethane PUR/UL VO
Glass parts Borosilicate glass 3.3 DIN/ISO 3585
Insulation steam generator Ceramic fiber Multitherm 550
Steam generator housing Stainless steel 1.4301
Protective door Polymethyl methacrylate PMMA
Seal ring Chlorosulfonyl polyethylene elastomer CSM
29
K-375/376/377 Operation Manual, Version B
3.6.3 K-376/K-377
Table 3-21: Material on the K-376/K-377
Part Material Material code
Housing (mounting plate) Steel sheet St 12 ZE 1.0330
Housing (casing-below) Stainless steel 1.4301 (L 314)
Housing (top cover) Alu-sheet AlMgSi1
Guide express rack PP PP
Coating Polyester/Epoxy PEP 31
Protective shield Polymethyl methacrylate/Alu PMMA/Alu
Drip tray Polypropylene PP
Housing y-axle Alu-sheet AlMgSi1
End cap y-axle POM POM
Dip tube PVDF PVDF
Sealing cap EPDM EPDM
Transfer hose linear PTFE PTFE
Steam tube Silicone/polyester MQ-PU
Protective hose PP PP
Hose chain PA PA
3 Technical data
30
K-375/376/377 Operation Manual, Version B
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