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K-360
User Manual
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BUCHI K-360 User Manual

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Operation Manual
KjelFlex K�360
093176
en
Table of contents
Table of contents
1.1 Abbreviations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
2.1 Safety warnings and safety signals used in this manual . . . . . . . . . . . . . . . . . 7
2.2 User qualification . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
2.3 Proper use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
2.4 Improper use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
2.5 Product safety. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
2.5.1 General hazards and safety measures. . . . . . . . . . . . . . . . . . . . . . . . . 10
2.5.4 Safety elements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
2.6 General safety rules . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
3 Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
3.1 Scope of delivery . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
3.1.1 Standard instrument. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
3.1.2 Standard accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
3.1.3 Optional accessories K-360 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
3.2 Technical data K-360 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
3.3 Titration solution. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
3.4 Reference substances. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
3.5 Materials used. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
4.1 Instrument overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
4.2 Function principle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
4.3 Kjeldahl applications. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
4.4 Non-Kjeldahl applications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
4.5 Operational elements of the instrument . . . . . . . . . . . . . . . . . . . . . . . . 22
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 instrument 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.
3 KjelFlex K-360 Operation Manual, Version C
Table of contents
5.1 Installation site. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
5.2 Electrical connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
5.3 Reagent and water connections. . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
5.3.1 Cooling water connection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
5.3.2 Drainage of cooling water . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
5.3.3 Waste/aspiration hoses . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
5.3.4 Storage tank connection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
5.4 Level sensors (optional) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
5.5 Connections to peripheral devices. . . . . . . . . . . . . . . . . . . . . . . . . . . 26
5.5.1 Connecting a printer. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
5.5.2 External keyboard . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
5.6 Boric acid titration and back titration . . . . . . . . . . . . . . . . . . . . . . . . . 28
6.1 Overview over the software structure . . . . . . . . . . . . . . . . . . . . . . . . . 30
6.2 General information on buttons . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33
6.3 Overview on how to prepare the instrument for routine operation . . . . . . . . . . . 34
6.3.1 Standard instrument configuration. . . . . . . . . . . . . . . . . . . . . . . . . . . 34
6.3.2 Distillation methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
6.3.3 System preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
6.3.4 Individual working method. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
6.4 Configuring the instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
6.4.1 Pump calibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36
6.4.2 Setting date and time . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36
6.4.3 Defining general instrument settings. . . . . . . . . . . . . . . . . . . . . . . . . . 37
6.4.4 Defining the titrator settings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
6.4.5 Boric acid / end point titration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38
6.4.6 Back titration with dispenser . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
6.4.7 Defining user and password settings . . . . . . . . . . . . . . . . . . . . . . . . . 39
6.4.8 Defining the keypad settings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40
6.5 Defining a distillation method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41
6.6 Instrument modes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
6.7 System preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
6.7.1 Preheating. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
6.7.2 Priming . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
6.7.3 Cleaning. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
6.7.4 Aspiration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
6.8 Carrying out a distillation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43
6.8.1 Single sample analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43
6.8.2 Rack oriented analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
6.8.3 Analysis screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
6.8.4 Result screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
6.8.5 Result list . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
6.8.6 After distillation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 46
6.9 Switching ON/OFF checklist. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 46
4
KjelFlex K-360 Operation Manual, Version C
Table of contents
7.1 Daily maintenance. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48
7.1.1 Cleaning the housing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48
7.1.2 Cleaning the glass parts. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48
7.1.3 Cleaning the rubber bung seal. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49
7.2 Monthly maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49
7.2.1 Calibrating the pumps . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49
7.2.2 Checking the distillate amount. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49
7.3 Maintenance as required . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49
7.3.1 Cleaning the splash protector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49
7.3.2 Replacing the splash protector . . . . . . . . . . . . . . . . . . . . . . . . . . . . 50
7.3.3 Replacing the rubber bung seals and the splash protector . . . . . . . . . . . . . . 50
7.3.4 Glass parts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52
7.3.5 Replacing the hoses. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52
7.4 Yearly maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 53
7.4.1 Customer service . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 53
7.4.2 Decalcification of the steam generator. . . . . . . . . . . . . . . . . . . . . . . . . 53
8.1 Malfunctions and their remedy. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54
8.2 Diagnostics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 56
8.2.1 Operational Tests . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 56
8.2.2 Test sensors. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57
8.2.3 Test Printer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57
8.2.4 Operating Hours. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57
8.2.5 Hardware Info . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57
8.2.6 Service Test . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57
9 Shutdown, storage, transport and disposal . . . . . . . . . . . . . . . . . . . . . . . . 58
9.1 Preparing the instrument for transport. . . . . . . . . . . . . . . . . . . . . . . . . 58
9.2 Storage and transport . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
9.3 Disposal. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
10.1 Spare parts K-360 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 60
10.2 Hosing connection schemes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62
11.1 FCC requirements (for USA and Canada) . . . . . . . . . . . . . . . . . . . . . . . 67
11.2 Declaration of conformity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 68
5 KjelFlex K-360 Operation Manual, Version C
1 About this manual
This manual describes the KjelFlex K-360 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 messages are explained in chapter 2.
1.1 Abbreviations
EPDM: Ethylene Propylene Dimonomer FCC: Federal Communications Commission FEP: Fluorethylene Propylene NBR: Nitrile Butadiene Rubber PE: Polyethylene PMMA: Polymethyl methacrylate PP: Polypropylene PTFE: Ethylenetetrafluoroethylene (Teflon) PUR: Polyurethane RSD: Relative Standard Deviation
1 About this manual
6 KjelFlex K-360 Operation Manual, Version C
2 Safety
!
This chapter points out the safety concept of the instrument 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 safety­related 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 Safety warnings and safety signals used in this manual
DANGER, WARNING, CAUTION and NOTICE are standardized signal words for identifying levels of hazard seriousness for 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 below table with the different signal words and their definitions!
2 Safety
Sign Signal word Definition Risk level
DANGER
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 below example).
Space for
supplementary
safety
information
symbols.
Supplementary text, describing the kind and level of hazard / risk seriousness.
•
•
•
Indicates a hazardous situation which, if not avoided, will result in death or serious injury.
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
List of measures to avoid the herein described, hazard or hazardous situation.•
״ ״ ״
★★★★
★★★☆
★★☆☆
★☆☆☆
(property damage only)
״ ״ ״
7 KjelFlex K-360 Operation Manual, Version C
2 Safety
Table of supplementary safety information symbols The below reference list incorporates all safety information symbols used in this manual and their
meaning.
Warning symbols Meaning
Electrical hazard
Hot machine parts, hot surface
Corrosive substances
General warning sign
General system damage
Mandatory action symbols Meaning
Wear safety gloves
Wear protective goggles
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 below example).
NOTE
Useful tips for the easy operation of the instrument / software.
8 KjelFlex K-360 Operation Manual, Version C
2.2 User qualification
The instrument 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.
2.3 Proper use
The instrument has been designed and built for laboratories. It serves for the distillation of steam-vola­tile substances.
2.4 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 instrument in rooms which require ex-protected instruments.• Use on samples, which can explode or inflame (e.g. explosives, etc.) due to shock, friction, heat or • spark formation.
2 Safety
2.5 Product safety
The instrument is designed and built in accordance with state-of-the-art technology. Nevertheless, risks to users, property and the environment can arise when the instrument is used carelessly or improperly.
The manufacturer has determined residual dangers emanating from the instrument
if the instrument is operated by insufficiently trained personnel.• if the instrument is not operated according to its proper use.•
Safety warnings in this manual (as discribed in section 2.1 ff) serve to make the user alert and to avoid hazardous situations emanating from residual dangers by giving appropriate counter meassured.
9 KjelFlex K-360 Operation Manual, Version C
2.5.1 General hazards and safety measures
!
!
WARNING
Death or serious injuries by explosive solvent atmosphere.
Operate the system in well ventilated environments only.• Do not use open flames in explosive environments.• Avoid eletrostatic and electric spark formation in explosive environments.•
WARNING
Death or serious injuries by strong corrosives.
Observe supplementary data sheets of all used chemicals.• Handle corrosives in well ventilated environments only.• Always wear protective goggles.• Always wear protective gloves.•
2 Safety
2.5.4 Safety elements
The instrument is provided with the following safety elements:
Protective door: Safety appliance to protect users from burns at the splash protector (distillation • area), which is hot during distillation. Protective door sensor: Prevents the start of a distillation with the protective door open and stops • a running distillation and the dosing of reagents immediately when the protective door is opened during the process. Sample tube sensor: Prevents the start of a distillation without a sample tube inserted.• Protective shield (cover) at condenser: Protects the glass parts.• Service door sensor/switch: Electrical power is disconnected immediately when the service door is • opened, thus preventing electrical shock during maintenance. Cooling water flow sensor: Stops a running distillation.• Optional level sensors for reagent and waste tank: A running distillation is interrupted when the • tanks are too full or too empty respectively. Drip tray: Collects overflowing liquids.• Automatic chemical dosage: Ensures the use of homogeneous liquid amounts.•
10 KjelFlex K-360 Operation Manual, Version C
2.6 General safety rules
Responsibility of the operator The head of laboratory is responsible for training his personnel.
The operator shall inform the manufacturer without delay of any safety-related incidents which might occur during operation of the instrument. Legal regulations, such as local, state and federal laws applying to the instrument must be strictly followed.
Duty of maintenance and care The operator is responsible for ensuring that the instrument is operated in proper condition only, and
that maintenance, service, and repair jobs are performed with care and on schedule, and by autho­rized personnel only.
Spare parts to be used Use only genuine consumables and genuine spare parts for maintenance to assure good system
performance and reliability. Any modifications to the spare parts used are only allowed with the prior written permission of the manufacturer.
2 Safety
Modifications Modifications to the instrument are only permitted after prior consultation with 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.
11 KjelFlex K-360 Operation Manual, Version C
3 Technical data
This chapter introduces the reader to the instrument specifications. It contains the scope of delivery, technical data, requirements and performance data.
3.1 Scope of delivery
Check the scope of delivery according to the order number.
NOTE
For detailed information on the listed products see www.buchi.com or contact your local dealer.
3.1.1 Standard instrument
3 Technical data
Table 3-1: Standard instrument
Product Order number
KjelFlex K-360 Standard with glass splash protector, 230 V, 50/60 Hz
KjelFlex K-360 Standard with splash protector made of fiber glass reinforced polypropylene, 230 V, 50/60 Hz
KjelFlex K-360 with glass splash protector and acid resistant pump, 230 V, 50/60 Hz
KjelFlex K-360 with splash protector made of fiber glass reinforced polypro­pylene and acid resistant pump, 230 V, 50/60 Hz
KjelFlex K-360 Standard with glass splash protector and titration set, 230 V, 50/60 Hz
KjelFlex K-360 with splash protector made of fiber glass reinforced polypro­pylene and titration set, 230 V, 50/60 Hz
KjelFlex K-360 with glass splash protector, acid resistant pump and titra­tion set, 230 V, 50/60 Hz
KjelFlex K-360 with splash protector made of fiber glass reinforced polypro­pylene, acid resistant pump and titration set, 230 V, 50/60 Hz
43600
43601
43605
43604
43607
43606
43609
43608
12 KjelFlex K-360 Operation Manual, Version C
3.1.2 Standard accessories
1
8
2
3 Technical data
Table 3-2: Standard accessories
Product Order number
Mains cable of the following types
Type CH 10010
Type Schuko 10016
Type GB 17835
Type AUS 17836
Type USA 33763
Type Japan 10016
a Pair of glass tongs 02004
7
6
b Cooling water hose complete: G ¾",
½", L = 1.5 m
c Hose cooling water drain, silicone,
3
4
5
L = 1.8 m, Ø 14/10 mm
d Weighing boats 40444
e Hose chemical supply, Solaflex,
37780
43439
43185
L = 6 m, Ø 10/5 mm
f 3 suction hoses to tanks, FEP,
43407
L = 580 mm
g Hose waste drain, EPDM,
43457 L = 1.8 m, Ø 18/11 mm for acid resistant pump
h Hose Viton (acid resistant),
43693 L = 1.2 m, Ø 6/3 mm (only supplied for instruments with acid resistant pump)
4 clamps Ø 11.9 43841
i 3 tanks 10 l, without caps 43410
j 1 cap for 10 l tanks, large 25869
9
k 12 tank labels 43434
11
10
12
l 1 cap for 10 l and 20 l tanks, small 43477
Operation Manual:
English 93176
German 93177
French 93178
Italian 93179
Spanish 93180
13 KjelFlex K-360 Operation Manual, Version C
3.1.3 Optional accessories K-360
1
7
2
5
3
6 8
3 Technical data
Table 3-3: Optional accessories K-360
Product Order number
a Sample tube (set of 4), 500 ml 43982
b Set of sample tubes (set of 4), 300 ml 37377
c Receiving vessel 420 ml 43390
4
d Receiving vessel 340 ml 43333
Tanks without level sensors, including caps
e 10 l chemicals 43468
e 10 l waste 43470
h 20 l chemicals 43469
h 20 l waste 43471
Tanks with level sensors, including caps
g 10 l chemicals 43472
g 10 l waste 43374
f 20 l chemicals 43473
f 20 l waste 43475
Indicator according to Sher, 100 ml 03512
External PC keyboard (US) 31456
External PC keyboard (D) 31457
External dosage device for back titration,
43367
115 V
External dosage device for back titration,
43596
230 V
Cable for external dosage device for back
43621
titration (Schott Titronic)
14 KjelFlex K-360 Operation Manual, Version C
3 Technical data
Table 3-3: Optional accessories K-360
Product Order number
Sample tube holder for 4 sample tubes,
16951
500 ml each
Holder for 6 sample tubes, 300 ml 43039
Holder for 12 sample tubes, 300 ml 43041
Titration set 43698
Splash protector for Devarda method 43335
Connection cable to: Mettler (DL15 / 22) titrator
Metrohm (785 / 719 / 702) Mettler (Txx) titrator
43616
43617
Metrohm (848) titrator 11055333
Schott titrator 43618
Radiometer titrator 43619
Adapter for Metrohm 719 / 702 47803
15 KjelFlex K-360 Operation Manual, Version C
3 Technical data
Table 3-3: Optional accessories K-360 (cont.)
Product Order number
SO2 accessory 48680
IQ/OQ set for K–360, English 93189
IQ/OQ set for K–360, German 45541
Repeating OQ, English 11055493
Repeating OQ, German 11055494
3.2 Technical data K-360
Table 3-4: Technical data K-360
Power consumption max. 2.2 kW
Connection voltage 220 - 240 VAC ± 10%
Frequency 50/60 Hz
Mains connection 3-pole (P, N, E) via power cord
Recovery rate ≥ 99.5%
Reproducibility (RSD) ≤ ± 1%
Detection limit ≥ 0.1 mg Nitrogen
Vapor output control 30 - 100%
Environmental conditions
Temperature Altitude Humidity
Installation category II
Pollution degree 2
Dimensions (W x H x D) 405 x 660 x 400 mm
Weight 22 kg
Printer interface USB 2.0, PCL 6
KjelFlex K-360
for indoor use only 5 - 35 °C up to 2000 m maximum relative humidity 80% for temperatures up to 31 °C decreasing linearly to 67% relative humidity at 35 °C
16 KjelFlex K-360 Operation Manual, Version C
3.3 Titration solution
The amount of sample and the concentration of the titrant should be optimized, so that the titrant volume is between 2 and 18 ml (burette volume: 20 ml).
Table 3-5: Titration solution 1
N-amount N-content Sample size Titrant Titrant concentration Titrant volume
5 mg N 0.5 % N 1 g
10 mg N 1.0 % N 1 g
50 mg N 5 % N 0.1 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
Table 3-6: Titration solution 2
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
H2SO H2SO H2SO H2SO H2SO H2SO H2SO
4
4
4
4
4
4
4
H2SO H2SO H2SO H2SO H2SO H2SO H2SO
3 Technical data
0.01 mol/l
0.05 mol/l
0.01 mol/l
0.25 mol/l
0.5 mol/l
0.5 mol/l 1 mol/l
4
4
4
4
4
4
4
0.01 mol/l
0.01 mol/l
0.1 mol/l
0.1 mol/l
0.25 mol/l
0.25 mol/l
0.5 mol/l
17.8 ml
7.1 ml
17.8 ml
14.3 ml
7.1 ml
14.3 ml
7.1 ml
11.42 ml
11.42 ml
5.71 ml
11.42 ml
4.57 ml
9.14 ml
11.42 ml
General recommendation Hydrochloric acid has the disadvantage of degassing. Therefore Buchi recommends to use sulfuric
acid as titrant. The correction factor for self prepared solutions is called a 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
3.4 Reference substances
Table 3-7: Reference substances
Name Purity % N theoretical
Ammonium dihydrogen phosphate
Glycine 99.7 18.66 0.5 g c(H2SO4) = 0.25
Phenylalanine 99.0 8.47 0.9 g c(H2SO4) = 0.25
Ammonium sulfate
99.5 12.18 0.8 g c(H2SO4) = 0.25
99.5 21.21 0.4 g c(H2SO4) = 0.25
(100 % purity)
Recommended
sample size
Recommended titrant
concentration
mol/l
mol/l
mol/l
mol/l
Digestion necessary
No
Yes
Yes
No
17 KjelFlex K-360 Operation Manual, Version C
3.5 Materials used
Table 3-8: Materials used for the K-360
Component Material designation Material code
Housing Polyurethane PUR / UL V0
Glass parts Borosilicate glass 3.3 DIN/ISO 3585
Steam generator isolation Ceramic fiber Multitherm 550
Steam generator housing Stainless steel 1.4301
Protective door Polymethyl methacrylate PMMA
Condenser cover Polymethyl methacrylate PMMA
Connecting stopper Hypalon CSM
Plastic splash protector Glass fiber reinforced polypropylene PP
Stop-cock Polypropylene/polyethylene PP/PE
3 Technical data
18 KjelFlex K-360 Operation Manual, Version C
4 Description of function
This chapter explains the basic principle of the instrument, shows how it is structured and gives a functional description of the assemblies.
4.1 Instrument overview
4
4 Description of function
1
2
3
a Splash protector b Sample tube c Protective door
Fig. 4.1: Instrument overview
5
6
d Condenser e Operating panel f Service door
19 KjelFlex K-360 Operation Manual, Version C
4.2 Function principle
The KjelFlex K-360 is suitable for determining nitrogen using the Kjeldahl (TKN; Total Kjeldahl Nitrogen) and Devarda methods as well as for other distillations of steam-volatile substances (e.g. of alcohol, SO2, volatile acids).
2
4 Description of function
a Sample tube
3
4
5
b Splash protector c Steam generator d Condenser e Distillate outlet tube f Receiving vessel with receiver solution
1
Fig. 4.2: Function principle
Steam is introduced into the sample solution (in sample tube a) to drive out volatile components (such as ammonia, alcohol, etc.). After condensation (in condenser d) the distillate is collected in a receiver solution (in receiving vessel f).
4.3 Kjeldahl applications
Determination of nitrogen/protein. For system configuration with reagent-pump: Warnmeldung
4.4 Non-Kjeldahl applications
Typical examples for non-Kjeldahl methods.
6
Determination of:
SO•
2
Phenol• Formaldehyde• TVBN• Alcohol• Volatile acids•
20 KjelFlex K-360 Operation Manual, Version C
4 Description of function
!
Fig. 4.3: Stop-cock
The stop-cock is located at the inside of the service door. To carry out a Kjeldahl application the stop-cock must be in downwards position. To carry out a non-Kjeldahl application the stop-cock must be in horizontal position.
CAUTION
Risk of burnings by hot machine parts and water steam.
Let the system cool down before performing any service.• Do not operate the instrument when enclosure is open or removed.•
Notice
Wrong stop-cock setting will result in system overpressure. Tubing may come off.
Set stop-cock to correct working-position.•
21 KjelFlex K-360 Operation Manual, Version C
4 Description of function
NOTE
A warning message will be displayed, when the method is changed from a Kjeldahl to a non-Kjeldahl method or vice versa:
Fig. 4.4: Warning message on the display Fig. 4.5: Warning message on the display
4.5 Operational elements of the instrument
1
3
3 3
2
3
4
5
a Stop button to stop a process b Display c Functional buttons to operate the software d Navigation buttons to navigate within the
software
e Start button to start a process like preheating,
priming, cleaning, etc.
f Enter button to move forward within the sub-
menu structure
g Escape button h Delete button to delete a digit entered via the
keypad
i Keypad
6
9
7
8
Fig. 4.6: Controls of the instrument
22 KjelFlex K-360 Operation Manual, Version C
5 Putting into operation
L
N
IEC-60320, Type: C13
!
This chapter describes how the instrument is installed and gives instructions on initial startup.
NOTE
Inspect the instrument for damages during unpacking. If necessary, prepare a status report immedia­tely to inform the postal company, railway company or transportation company.
Keep the original packaging for future transportation.
5.1 Installation site
Install the instrument on a clean, flat and stable base and place the tanks for chemicals beside the instrument (not higher and not more than 1 m lower).
Notice
Reduced instrument safety and lifetime due to improper handling and installation location.
Do not place any object on top of the instrument.• Keep a free safety space of 30 cm around the instrument.• Do not place items behind the instrument.• Do not operate the instrument within an fume cabinet.•
5 Putting into operation
5.2 Electrical connections
Fig. 5.1: Electrical connections
Death or serious burnings by electric shock.
Mains voltage must match the voltage reading on the type plate.• Instrument must be earthed by the mains socket.• Only use a molded 3-pole device plug (IEC-60320, type C13 or C15).• Do not use damaged cables.•
WARNING
23
KjelFlex K-360 Operation Manual, Version C
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