Knauer 4000 MiD Mode d'emploi

Mass spectrometer

Instructions

Document No. V6695

HPLC

4000 MiD®

4000 MiD® Instructions, V6695

Table of contents

Note: For your own safety, read the instructions and observe the

warnings and safety information on the device and in the instructions.

Keep the instructions for future reference.

Phone: +49 30 809727-111 (9-17h, Central European Time)

Fax: +49 30 8015010

E-Mail: support@knauer.net

Languages: German, English

KNAUER Wissenschaftliche Geräte GmbH

Hegauer Weg 38

D-14163 Berlin

Phone: +49 30 809727-0

Fax: +49 30 8015010

Internet: www.knauer.net

E-Mail: info@knauer.net

Version information: Article number: V6695

Version number: 1.0

Last update: 2018/08/21

Copyright: This document contains conﬁdential information and may not be

reproduced without written content of KNAUER Wissenschaftliche

Geräte GmbH.

Technical Support:

Publisher:

The information in this document is subject

to change without prior notice.

For latest version of the instructions, check our website:

https://www.knauer.net/en/Support/User-manuals

4000 MiD® Instructions, V6695

Table of contents

1. Symbols and signs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1

1.1 Terms and abbreviations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1

1.2 Warning symbols (ENG) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1

1.3 Pictogrammes de sécurité (FRA). . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2

2. Important safety information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4

2.1 Electrical hazards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4

2.2 Chemical hazards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5

2.3 Compressed gas hazards. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5

2.4 Safety and regulatory standards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6

2.4.1 Electromagnetic compatibility . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7

2.4.2 Precautions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7

3. Product information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9

3.1 Theory of microspray . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10

3.2 Views . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10

3.2.1 The front panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10

3.2.2 LED status indicators. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11

3.2.3 The rear panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12

4. Scope of delivery. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13

5. Unpacking and setup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

5.1 Site requirements and storage conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

5.2 Power supply . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

5.3 Power cords . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

5.4 The MiD and associated parts. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15

5.5 Setting up the MiD . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16

5.5.1 Operational conﬁguration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17

5.5.2 The rear panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17

5.5.3 Switching on the system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18

5.5.4 The source, ﬁlter, detector (SFD) assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . 19

5.6 The spraychip ﬂange. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19

5.7 The vac-chip assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20

5.8 The spraychip assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22

5.8.1 The Split Flow Interface (SFI) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23

5.8.2 The Direct Flow Interface (DFI) – optional . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25

5.8.3 Installing spraychip assemblies . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25

5.8.4 Operating the front cover safety interlock . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26

5.8.5 Installing a syringe pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27

6. Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .28

6.1 Preparing to analyse . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28

6.1.1 MiD system pump-down . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28

4000 MiD® Instructions, V6695

Table of contents

6.2 Shutting down the MiD. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28

6.2.1 Entering ‘Standby’ mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28

6.2.2 Venting the MiD . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28

6.2.3 Shutting down the MiD . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28

7. Functional tests . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .29

7.1 Installation Qualiﬁcation (IQ) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29

7.2 Operation Qualiﬁcation (OQ) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29

8. Calibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .30

8.1 Installing the calibration kit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30

8.2 Calibration routine . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30

8.3 Flushing the system after calibrating . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31

9. Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31

9.1 General maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31

9.2 Removing and replacing the spraychip . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33

9.3 Cleaning the spraychip. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34

9.3.1 Cleaning the Spraychip with DFI . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34

9.3.2 Cleaning the Spraychip with SFI . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34

9.4 Liquid ﬂow rate measurement. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35

9.5 Spraychip assembly cleaning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36

9.5.1 Cleaning the Direct Flow Interface . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36

9.5.2 Cleaning the Split Flow Interface. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37

9.6 Spraychip assembly maintenance. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38

9.6.1 Replacing the Direct Flow Interface tubing . . . . . . . . . . . . . . . . . . . . . . . . . . . 38

9.6.2 Replacing the Split Flow Interface tubing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40

9.7 Removing and replacing the vac-chip . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42

9.8 Cleaning the vac-chip . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45

9.9 Cleaning the vac-chip ﬂange . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 46

10. Troubleshooting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47

11. Technical data. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .50

12. Reorder . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 50

Appendices . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51

1

4000 MiD® Instructions, V6695

1. Symbols and signs

1.1 Terms and abbreviations

Term Deﬁnition

ESI Electrospray Ionisation

LC Liquid Chromatography

DFI Direct Flow Interface

SFI Split Flow Interface

MiD Molecular iD

m/z ratio Mass-to-charge ratio

MSDS Material Safety Data Sheet

RF Radio Frequency

SFD Source, Filter, Detector (assembly)

TIC Total Ion Current

1.2 Warning symbols (ENG)

The warning symbols described in the table below are used on the MiD

and within these Instructions. All warnings and cautions must be obser-

ved at all times during operation and maintenance of the MiD. Failure to

comply with the warning instructions violates safety standards associated

with the proper use of the system and its design. KNAUER assumes no

liability for the failure to comply with these requirements.

Symbol Description

Alternating Current

Conformité Européenne

Read the Instructions

C

A Safety Alert symbol with the C notice de-

notes a potential hazard. Pay particular attention to

the procedure or operation described. If performed

incorrectly or without caution, the procedure may

result in damage to hardware or the software.

DO NOT proceed beyond a C notice without

fully understanding the notice, its implications and

how to meet the conditions stated.

Symbols and signs

2

4000 MiD® Instructions, V6695

Symbol Description

W S H

A Safety Alert symbol with the W notice de-

notes a serious hazard. The operation or suggested

action may result in personal injury or death.

DO NOT proceed beyond a W notice wit-

hout fully understanding the notice, its implications

and how to meet the conditions stated.

Warning notices are also displayed with symbols

representing speciﬁc hazards.

C,    

This symbol denotes a risk of electric shock. It indica-

tes areas on the MiD system where hazardous vol-

tages are present.

W H V

This symbol highlights actions or procedures which,

if not performed correctly, could lead to electric

shock from hazardous voltages.

W C C

This symbol with the W notice denotes

corrosive chemicals. A corrosive chemical may be

present. Exposure may result in serious injury. Use

appropriate skin protection.

Note: A Note indicates important information necessary for the correct

or optimal operation of the software or hardware. Read the information

carefully and follow any instructions.

1.3 Pictogrammes de sécurité (FRA)

Les pictogrammes de sécurité présents dans la table en dessous sont uti-

lisés sur le MiD et dans ce guide.  et  doivent

êtres suivit en tout temps lors de l’entretien, l’installation, la réparation et

l’opération du MiD. Tous default d’application de ces règles de sécurité

serait considéré comme une violation des normes de sécurité. KNAUER

ne saurait voir sa responsabilité engagée en cas de manquement de l’uti-

lisateur à respecter les consignes de sécurité.

Symbole Description

Courant Alternatif

Conformité Européenne

Lisez le Guide de l’utilisateur

Symbols and signs

3

4000 MiD® Instructions, V6695

Symbole Description

A

Un symbole de sécurité avec la mention A

dénote un risque potentiel. Soyez particulièrement

attentif à la procédure décrite. Si celle-ci est exécu-

tée de manière incorrecte, elle peut engendrer un

dommage de l’équipement et/ou une erreur de pro-

gramme avec la conséquence probable de perdre

des données.

Ne continuer pas après un signal d’A sans

comprendre totalement sa signiﬁcation et les condi-

tions décrites.

A   

Un symbole de sécurité avec la mention A-

 dénote un danger sérieux. La procédure

décrite peut entrainer un risque de blessure ou de

mort.

Ne continuer pas après un signal d’A

sans comprendre totalement sa signiﬁcation et les

conditions décrites.

Des notices d’avertissement sont aussi associées

avec des pictogrammes représentant des dangers

spéciﬁques.

A,    

Ce pictogramme dénote la possibilité de choc élec-

trique. Ce pictogramme peut êtres trouvé sur le MiD.

Il indique une région du MiD où des tensions électri-

ques sont présentes.

A   

Ce pictogramme avec la mention A

dénote des tensions dangereuses. Ce pictogramme

peut êtres trouvé sur le MiD. Il indique une région du

MiD ou des tensions dangereuses sont présentes.

A   

Ce symbole met en évidence des actions ou des

procédures qui, si elles ne sont pas eectuées cor-

rectement, peut entraîner l’exposition à des substan-

ces corrosives. Utilisez des protections corporelles

adéquates.

Note: Une Note indique des informations importantes pour l’utilisation

du software et/ou de l’équipement. Veuillez lire les informations avec

attention et suivez les instructions.

Symbols and signs

4

4000 MiD® Instructions, V6695

Units

Imperial and metric units.

Both imperial and metric units are used in this document. The unit of

measurement chosen reﬂects historical use. Please note that the unit sym-

bol for inches is given as ˝; for example: 6˝ means 6 inches.

Pressures in the vacuum system of the MiD are measured in Torr. For

example, a typical pressure reading in the user interface of the software

would be 2.0 E-5 Torr: this is equivalent to 2.0×10-5 Torr.

2. Important safety information

The safety information given in this section is important; always observe

all safety precautions when operating, maintaining, or servicing the 4000

MiD®.

To avoid personal injury or damage to the instrument, DO NOT perform

servicing or maintenance unless you are qualiﬁed and authorised to do

so. DO NOT perform any servicing or maintenance procedures that are

not described in these Instructions.

W If the equipment is used in a manner not speciﬁed by

the manufacturer, the protection provided by the equipment may

be impaired.

A Si l’équipement est utilisé d’une manière non

spéciﬁée par le fabricant, la protection fournie par l’équipement

peut être altérée.

C The MiD should only be used with accessories that meet

the manufacturers speciﬁcations. Failure to do so may result in

damage to the instrument and lead to the loss of liability and war-

ranty entitlements.

A Le MID ne doit être utilisé qu’avec les accessoires qui

répondent aux spéciﬁcations du fabricant. Le cas contraire peut

causer des dommages à l’appareil et entraîner la perte de respon-

sabilité et de droits de garantie.

2.1 Electrical hazards

Dangerous high voltages

Several internal parts of the MiD can supply dangerous voltages. When

the MiD is connected to the mains supply dangerous high voltages can

be present even if the power is switched o.

W Unless speciﬁcally instructed, DO NOT remove any

protective covers. The product is sealed at the factory. Damage

or removal of the warranty seals leads to the loss of liability and

warranty entitlements.

A Sauf mention contraire, NE PAS retirer les cou-

vercles de protection. Le produit est scellé à l’usine. Les dom-

mages ou levée des scellés de garantie entraîne la perte de la

responsabilité et droits de garantie.

Symbols and signs

5

4000 MiD® Instructions, V6695

2.2 Chemical hazards

Any chemicals used for analysis should be handled according to good

laboratory practice. They should also be stored, used, and disposed of

in accordance with the manufacturer’s speciﬁcations, as well as local and

national regulations.

The responsible individual must ensure that personnel are not exposed

to hazardous levels of toxic substances as outlined in the Material Safety

Data Sheets (MSDS), or any documentation provided by local governing

bodies such as The Health Protection Agency (UK) or The Occupational

Safety and Health Administration (US).

W Potentially hazardous chemicals can be used with the

MiD. Use care when handling chemicals and wear appropriate

PPE.

A Des produits chimiques potentiellement dange-

reux peuvent être utilisés avec le MiD. Faire preuve de prudence

lors de la manipulation des produits chimiques et porter des EPI

appropriés.

W The pump exhausts from the MiD must be connected

to a suitable extraction system. Appropriate extraction must also

be provided to the microspray area when analysing hazardous

chemicals.

A Les gaz d’échappement de la pompe du MiD

doit être connecté à un système d’extraction approprié. Une

extraction adéquate doit également être fournie à la zone micros-

pray lors de l’analyse de produits chimiques dangereux.

C This system operates using high voltages. This can intro-

duce additional hazards when certain solvents are used. Ensure all

solvents and instruments are properly connected, vented, or set

up with manufacturer approved settings.

A Ce système fonctionne avec des tensions électriques

élevées. Cela peut présenter des dangers supplémentaires

lorsque certains solvants sont utilisés. S’assurer que tous les sol-

vants et les instruments sont correctement connectés, ventilé, ou

mis en place avec les paramètres homologués par le constructeur.

2.3 Compressed gas hazards

The MiD requires a source of dry nitrogen gas for correct operation.

Always follow local health and safety regulations if handling cylinders of

compressed gas. Environmental monitoring must be deployed to detect

and alert the user to the occurrence of a reduction of oxygen due to a ni-

trogen leak in the environment. In case of oxygen reduction, all personnel

need to leave the room and alert the proper health and safety represent-

ative.

Symbols and signs

6

4000 MiD® Instructions, V6695

2.4 Safety and regulatory standards

In accordance with the following directives:

2006/95/EC

The Low Voltage Directive

2004/108/EC

The Electromagnetic Compatibility Directive

The MiD complies with the following safety standards:

IEC 61010-1: 2010 (3rd Edition)

Safety requirements for electrical equipment for measurement, cont-

rol, and laboratory use.

UL 61010-1: May 2012

Electrical Equipment for Measurement, Control, and Laboratory Use;

Part 1: General Requirements.

CSA C22.2 61010-1 (3rd Edition - 2011)

Safety Requirements for Electrical Equipment.

The MiD conforms to the following standards for EMC conformity:

IEC/EN 61326:2006

Electrical equipment for measurement, control and laboratory use

EMC requirements.

EN 61000-3-2:2006 + A1:2009 + A2:2009

Electromagnetic compatibility (EMC).

Limits for harmonic current emissions

(equipment input current < 16 A per phase).

EN 61000-3-3:2008

Electromagnetic compatibility (EMC).

Limitation of voltage changes, voltage ﬂuctuations and ﬂicker in public

low-voltage supply systems, for equipment with rated current ≤ 16 A

per phase and not subject to conditional connection.

ICES-003:2004

Spectrum Management and Telecommunications Policy.

Interference-Causing Equipment Standard.

Digital Apparatus.

In accordance with all of the essential requirements of

all applicable European product directives; the decla-

ration of conformity document is available upon

request.

FCC CFR47:Part 15:B:2008

Note: This equipment has been tested and found to comply with the

limits for a Class A digital device, pursuant to part 15 of the FCC Rules.

These limits are designed to provide reasonable protection against

harmful interference when the equipment is operated in a commercial

environment. This equipment generates, uses, and can radiate radio

frequency energy and, if not installed and used in accordance with the

instruction manual, may cause harmful interference to radio communicati-

ons. Operation of this equipment in a residential area is likely to cause

harmful interference in which case the user will be required to correct the

interference at their expense.

Symbols and signs

7

4000 MiD® Instructions, V6695

Modiﬁcations not expressly approved by the manufacturer could void the

user’s authority to operate the equipment under FCC rules.

Subject to the Waste Electrical and Electronic Equipment (WEEE)

Directive; see WEEE compliance statement.

WEEE Compliance Statement

This statement is valid only for customers in EU member countries. The

European Union (EU) directive for product recycling (The Waste Electri-

cal and Electronic Equipment - WEEE Directive) will shortly be incorpo-

rated into the national laws of each EU member state. Products falling

under the scope of the WEEE Directive are identiﬁed with a crossed over

“wheelie” bin symbol on the product label. An authorized waste disposal

service must be used to dispose of the product for recycling or disposal,

or alternatively return the product to KNAUER.

W The manufacturer’s declaration becomes invalid if the

user modiﬁes the original product or installs additional compo-

nents.

A La déclaration du fabricant est annulée si l’uti-

lisateur modiﬁe l’origine du produit ou installe des composants

supplémentaires.

2.4.1 Electromagnetic compatibility

The manufacturer has tested and evaluated the MiD to ensure it fully

complies with EMC and safety standards as outlined in IEC 61010-1:

2010.

2.4.2 Precautions

The following safety precautions concerning the operation of the MiD

and the site in which it is used must be observed at all times in order to

prevent injury and damage to the system and associated instruments.

W At least two people are required to lift or move the

MiD.

A Au moins deux personnes sont nécessaires

pour soulever ou déplacer le MiD.

W To prevent injury and damage to equipment please

ensure the blanking plug is removed from the exhaust port before

activating the pumps.

A Pour éviter blessures et dommages matériels,

veuillez vous assurer que le bouchon de fermeture soit retiré de

l’oriﬁce d’échappement avant d’activer les pompes.

Symbols and signs

8

4000 MiD® Instructions, V6695

W DO NOT use the instrument if there are signs of visible

damage.

DO NOT operate if site conditions are not within speciﬁcations.

DO NOT override any safety interlock.

A NE PAS faire fonctionner l’appareil s’il présente

des signes de dommages visibles.

NE PAS faire fonctionner si les conditions du site ne sont pas

conformes aux spéciﬁcations.

NE PAS altérer un verrouillage de sécurité.

W DO NOT attempt to operate the instrument with the

covers removed. High voltages are present when the instrument is

in operation.

DO NOT attempt to adjust or replace components other than

those that have been described in these Instructions.

A NE PAS essayer de faire fonctionner l’appareil

avec les couvercles enlevés. Des hautes tensions sont présentes

lorsque l’appareil est en fonctionnement.

NE PAS tenter de régler ou remplacer des composants autres que

ceux qui ont été décrits dans ce Guide de l’utilisateur.

W The instrument is not designed to be operated in a

potentially explosive atmosphere. It is the responsibility of the

customer to verify the operating environment meets the require-

ments of a “non-hazardous area” with regards to potentially explot-

sive atmosphere.

A L’instrument n’est pas conçu pour être utilisé

dans une atmosphère explosible. Il est de la responsabilité du

client de vériﬁer que l’environnement de fonctionnement répond

aux exigences d’un secteur non-dangereux quant à l’atmosphère

explosible.

Symbols and signs

9Product information

4000 MiD® Instructions, V6695

3. Product information

Note: Only use the device for applications that fall within the range of

the intended use. Otherwise, the protective and safety equipment of the

device could fail.

The 4000 MiD® is a compact mass detector system that employs mi-

cro-engineering technology to identify the chemical contents of solu-

tions.

The MiD incorporates technologies patented by Microsaic Systems plc

including; spraychip®, vac-chip™, and ionchip®.

A chemical sample, dissolved in suitable solvents, is introduced into the

spraychip, typically from an HPLC or syringe pump. Gas phase ions are

formed and are introduced into the vacuum chamber through the vac-

chip.

The ions introduced through the vac-chip are then focused using a series

of electrostatic ion optics. The ionchip ﬁlters the ions according to their

mass-to-charge (m/z) ratios and directs them to the detection system.

The spraychip ion source

The spraychip is a micro-electrospray ion source. Compared to conven-

tional electrospray ion sources, microspray provides the following advan-

tages:

Increased ionisation eciency

Lower ﬂow rates, which means analysis of very small sample volumes

(for example, nanolitres) over long periods of time.

Very low solvent consumption and minimum waste, when coupled to a

nano-LC.

Lower voltages are required to provide ecient electrospray.

The spraychip can be coupled to nano-ﬂow systems (without a ﬂow

split) or to traditional LC systems (using a ﬂow splitter).

The vac-chip and ion optics

The vac-chip interface allows the MiD to achieve the operating pressures

required for analysis and it aids transportation of ions from the micros-

pray source into the vacuum system of the MiD.

Behind the vac-chip, there is a series of ion optics: a tube lens, an exit

lens, an ion guide and an inter-quadrupole lens. Ions generated from the

spraychip enter the vac-chip and are focused into the ionchip using the

ion optics.

The ionchip

The ionchip is a micro-engineered quadrupole mass analyser. It functions

like a conventional quadrupole mass analyser, acting as a mass ﬁlter,

separating ions in order of their mass-to-charge (m/z) ratios. However, it

is about one hundredth the volume of a conventional quadrupole mass

analyser.

Vacuum system

The vacuum system consists of a vacuum chamber coupled to two tur-

bo-molecular pumps, which are backed by a small diaphragm pump. All

vacuum pumps are integrated within the MiD. Unlike conventional mass

spectrometers there are no external, ﬂoor-standing rotary pumps. This

10 Product information

4000 MiD® Instructions, V6695

signiﬁcantly reduces the equipment noise, footprint, and size. This also

eliminates complications associated with rotary pumps, such as back-

stream of pump oil and the added expense of purchasing an oil trap.

The vacuum system comprises three sections:

The vac-chip interface

The ion guide chamber

The analytical chamber

The pressures in the chambers are monitored using Pirani gauges which

also act as high-voltage interlocks. These gauges turn o any high volta-

ges if the pressure readings in the chambers are above a set safety value.

3.1 Theory of microspray

Microspray is a soft ionisation technique. A voltage, generally between

0.7 and 1.5 kV, is applied to an analyte dissolved in a suitable solvent;

generally a mixture of water and an organic solvent. The solvent passes

through an emitter or capillary tip at a ﬂow rate of 300-1000 nL/min. The

voltages and ﬂow rates used in microspray are lower than for convention-

al electrospray ionisation. This means that lower volumes of sample and

solvent are consumed by the MiD. When coupled with a nano-ﬂow LC,

solvent consumption is reduced by several orders of magnitude when

compared to traditional HPLC systems.

Under the correct conditions, a plume of charged aerosol droplets forms

from a Taylor cone. Gas-phase analyte ions are subsequently formed from

these aerosol droplets. Ions produced by this method can have single

or multiple charges. Generally, high molecular weight compounds, for

example, proteins, produce a series of multiply-charged ions.

3.2 Views

3.2 .1 The front panel

Fig. 1 shows the connections and ports on the front panel of the MiD.

Refer to the labels listed in the table below during operation.

Connection Description

K USB Port

L On/O Power switch

M LED Status Indicators

N Spraychip assembly high voltage connection

11Product information

4000 MiD® Instructions, V6695

Fig. 1 Front panel connections

3.2.2 LED status indicators

There are four LED status indicators on the front panel of the MiD (see

M - Fig. 1). They are used to indicate the current operational status of the

instrument; the LEDs are shown in detail in Fig. 2.

Fig. 2 LED status indicators

The LEDs indicate the following statuses:

Red: Indicates that a serious error has occurred. User intervention will

be required to rectify the fault. Fault details will be displayed on via error

Door open

N

M

L

K

Door shut

yellow green

orange red

12 Product information

4000 MiD® Instructions, V6695

dialog in the software. The LED will not be reset until the application is

restarted, which is also required to conﬁrm the fault has been remedied.

Orange: Indicates that the MiD is acquiring data (mass scanning). The

LED will not be lit unless the MiD is scanning, for example it will not be lit

when a start or stop time is in eect.

Green: The hardware interlock is engaged when the LED is lit and vice

versa, see „5.8.4 Operating the front cover safety interlock“ on page 26

for more details.

Yellow: Indicates that the MiD is in operate mode, when unlit the MiD is in

standby.

3.2.3 The rear panel

Fig. 3 shows the connections and ports on the rear panel of the MiD.

These ports include terminals and connectors for the gas supply, vacuum

exhaust system and computer peripherals.

Refer to the labels listed in the table below when connecting the MiD and

any associated instruments.

W The 4000 MiD provides double/reinforced insulation

to mains circuits. Any external equipment that is connected to the

4000 MiD through the rear panel must itself also provide double/

reinforced insulation to the mains supply.

A Le 4000 MiD ore une double isolation renfor-

cée pour l’alimentation secteur. Tout équipement externe connec-

té aux 4000 MiD par le panneau arrière doit lui aussi fournir une

double isolation renforcée à l’alimentation secteur.

Connection Description

A Nebuliser Gas Port

B Aux I/O Port

C VGA Monitor Port

D RS232 Port

E 4x USB Ports

F 2x Ethernet Ports

GPump exhaust

HMain power

I PS/2 Ports

JeSATA Port

K HDMI Port

13Product information

4000 MiD® Instructions, V6695

Fig. 3 Diagram of rear panel

4. Scope of delivery

Note: Only use original parts and accessories made by KNAUER or a

com pany authorized by KNAUER.

4000 MiD

MiDas

Starter kit:

- Mains leads (2 in total)

- PTFE tubing (form Nitrogen input)

- Exhaust Silencer

- Split ﬂow interface

Tool kit

Valid documents:

Instructions (English)

Declaration of conformity

B

A

C

DJK

IFE

G

H

14 Product information

4000 MiD® Instructions, V6695

5. Unpacking and setup

5.1 Site requirements and storage conditions

The chapter „9. Troubleshooting“ on page 47 describes the site require-

ments and storage conditions necessary for the MiD. Make sure all the

requirements are met before installation and use of the system.

5.2 Power supply

The power supply in the MiD accepts any line voltage in the range

100–240 V. There is no voltage selector at the rear of the MiD and there

are no externally accessible fuses.

C When operating MiD it must be possible to disconnect

the instrument from mains supply at any time. In the event of an

emergency the power connector of the instrument must be easily

accessible and removable.

A Lors de l’utilisation MiD il doit être possible de décon-

necter l’appareil de l’alimentation secteur à tout moment. En cas

d’urgence, le connecteur d’alimentation de l’instrument doit être

facilement accessible et débranchable.

C When installing or operating the instrument you must

ensure that there is sucient space behind the instrument to un-

plug the power cord.

A Lors de l’installation ou l’utilisation de l’instrument vous

devez vous assurer qu’il ya susamment d’espace derrière l’appa-

reil pour débrancher le cordon d’alimentation.

5.3 Power cords

Power cords are available for the MiD depending on the country/region

of operation. The female end of all supplied power cords are identical

and plug into the rear of the instrument (see Fig. 3). The male end of the

cord will ﬁt the wall outlet of the appropriate country/region.

W The MiD must never be operated from a power outlet

that has no ground connection. The absence of a ground connec-

tion can lead to electric shock or short circuit.

A Le MID ne doit jamais être utilisé à partir d’une

prise de courant qui n’a pas de connexion à la terre. L’absence de

mise à la terre peut provoquer un choc électrique ou un court-cir-

cuit.

W Never use a power cord other than that supplied by

the manufacturer. The use of an inadequately rated power cord

can lead to electric shock or short circuit.

A N’utilisez jamais un cordon d’alimentation autre

que celui fourni par le fabricant. L’utilisation d’un cordon d’ali-

mentation non-adéquat peut provoquer un choc électrique ou un

court-circuit.

15Product information

4000 MiD® Instructions, V6695

W Never use any cabling not supplied or recommended

the manufacturer. Use of unspeciﬁed cabling may lead to improp-

er operation or failure to comply with safety or EMC regulations.

A Ne jamais utiliser des câbles non fournis ou

recommandés par le fabricant. L’utilisation de câbles non spéciﬁé

peut entraîner un mauvais fonctionnement ou du non-respect de

la sécurité ou de la compatibilité électromagnétique.

5.4 The MiD and associated parts

The following tables list the parts that are available with the MiD and their

part numbers. These numbers can also be used to order any replacement

items that are required.

Note: Part numbers and kit contents are subject to change.

C All items listed must only be supplied by the manufac-

turer or an agent thereof. Use of alternative parts may lead to

improper operation of the MiD or failure to comply with safety or

EMC regulations.

A Tous les articles énumérés ne doit être fourni que par

le fabricant ou un agent de celle-ci. L’utilisation de pièces alterna-

tives peut conduire à un mauvais fonctionnement du MID ou un

manquement à la sécurité ou de la compatibilité électromagné-

tique.

Part number Description of part

A66916 Calibration kit - containing

Plug 1/32“ ﬁngertight

Tubing sleeve, 1/16“ OD

Syringe adapter ﬁtting, 1/16“ OD

PEEK tubing – 1/32“ OD x 0.007“ ID

Syringe adapter

Syringe pump power supply

New Era (NE-1000) syringe pump

250 µL luer lock syringe

Syringe pump communication cable

Part number Description of part

A66907 vac-chip O-ring kit

A66908 vac-chip screw kit

A66919 SFI/DFI tubing & ferrule kit

Calibration kit

Optional

accessories

16 Product information

4000 MiD® Instructions, V6695

Part number Description of part

A66915 Tool kit – containing

0.8 x 4.5 x 125 mm ﬂat screwdriver

2.5 mm allen key – ‘T’ Handle

4 mm allen key – ‘T’ Handle

Size PH1 Phillips screwdriver

Delrin tweezers – ﬂat, round

SFD cover plate and dust cap

5.5 Setting up the MiD

Fig. 4 shows a typical conﬁguration of the 4000 MiD.

Fig. 4 The 4000 MiD

C Allow sucient spacing around the MiD for proper

cooling and for the connection of mains plug, gas inlets, syringe

pump, HPLC etc.

A Laissez un espace susant autour du MiD pour un

refroidissement correct et pour le raccordement de la prise de

courant, des entrées de gaz, de la pompe à seringue, HPLC, etc.

Tool kit

253 mm

354 mm

109 mm

449 mm

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