Maintenance work

 

Beschreibung: Beschreibung: Beschreibung: Beschreibung: Fid_Real

FID Cross section

 

Disassembling the FID

 

There are two reasons for taking a FID apart:

  1. Cleaning the FID from deposits after having used the GC for an extended period of time.
  2. Measuring gas flows of carrier gas, hydrogen and air.

 

Necessary tools are included in delivery. Procedure:

·           Turn off power, pull mains plug and close gas valve at the pressure gas cylinder.

·           Loosen socket set screw (2) and pull out the upper feeler (3). Loosen top screw (1) and take off upper section of the FID (13)

·           Same way remove the lower feeler (8) by loosening screw (7).

·           Turn out the two hexagon screws (not visible in Fig.) located on top of the center section (11), and take off center section.

·           Now the nozzle (9) can be removed by carefully turning it by hand. The flange can be removed with an open end wrench size 8 mm.

·           If necessary. loosen the screw (12) sideways the upper section and pull out the isolator and the collector electrode.

 

Disassembling the FID step by step:

Disassembling the FID

 

 

To assemble the FID repeat the steps above in reverse order. The connecting leads are marked: the cable with a red ring is to be connected to the upper feeler (3).

 

Important Note: Please take utmost care as to first mount the center section before pushing in and fastening the feeler (8). The same applies to the upper feeler (3). First mount the collector electrode (6) before inserting the feeler.

Beschreibung: Beschreibung: Beschreibung: Beschreibung: Fid_Warnung_01

 

Mounting the feelers

 

 

Cleaning the detector

All parts of the detector, except for the feelers, are very robust and can be cleaned mechanically with cleaning agents. Do not wet the feelers!

 

 

 

FID:   Adjusting gas flows

 

Applies only for Chromatographs equipped with flame ionisation detector.

 

Factory settings:      Nominal gas flows for FID:

Clean air gas flow:     v(air)  = 300 ml/min
Hydrogen gas flow:    v(H2)   =   30 ml/min

These values are factory preset for a hydrogene pressure of  0.3 bar  (4.35 psi).

Working with a different FID hydrogen pressure from the above one requires readjustment of hydrogen gas flow. It is recommended to check for correct gas flows from time to time, in any case this has to be done if the FID does not work as expected, for example if ignition is not taking place or the hydrogen valve has been manipulated inadvertently.

 

Preparation

 

·           Turn off GC. If the FID is still hot, wait until it can be touched by hand. Turn on the GC. After start up a message window appears. Select ‘Measure gas flow’ and the FID heating will stay turned off.

·           Completely disassemble the FID as described here. Remove the flange and the nozzle.

 

 

Measurement and adjustment of air flow

 

Beschreibung: Beschreibung: Beschreibung: D:\_CGA21_Manual\_Bilder\Bild 35 FID_Gasflow\Messung_Luft_FID.jpg

 

Measuring air flow at the FID

 

Screw the connector (included) into the right boring of the detector block. Slide the silicon hose that leads to the bubble flow meter over the connector tubing and measure the gas flow as described here Adjust the valve „Air“ until the gas flow is between 280 and 320 ml/min. Usage of the bubble flow meter is explained here

 

 

Measurement and adjustment of hydrogen gas flow at the FID

 

Measuring hydrogen and carrier gas flow at the FID

 

 

 

 

 

 

Measurement of carrier gas flow (gas flow through the capillary column)

 

 

The carrier gas flow should be known to compute and adjust the split ratio. The measuring set-up is the same as in the previous section, but the procedure is different. Advice: It is a whole lot simpler to compute the carrier gas flow or take the values from tables. See last chapter

 

 

WLD:            Measuring and adjusting the carrier gas flow

 

Connect the exit of the carrier gas from the TCD (Thermal Conductive Detector) with the bubble flow meter by sliding the silicon hose that leads to the bubble flow meter over the connector tubing.

 

Adjust the pressure regulator at the gas cylinder to approx. 0.2 bar and wait 1-2 minutes to allow the carrier gas to displace the air in the system. Carrier gas flow should be between 10 and 50 ml/min. See chapter 5.5.3 for more information about carrier gas flow and separation efficiency. Usage of the bubble flow meter is explained here.

 

 

 

FID: Adjusting the split ratio        

 

General remarks

 

Capillary columns can only separate small amounts of substances. Using normal microliter syringes it is not practical to inject smaller amounts than approx. 0.5 µl. Such being the case the amount of substance is once again reduced inside the injector in an adjustable ratio termed ’split ratio’. See chapter 4 for details. The split ratio represents the ratio between the amount of carrier gas entering the column and the amount leaving the injector unused through the so-called split vent. Split ratios from 1:5 to 1:200 are used. The ratio implies a tradeoff between sensitivity and separation efficiency that depends also from the type of column.  In our case values of around 1:20 to1:50 are a good compromise.

 

 

Example:

 

The following describes the adjustment of a split ratio of 1:50

·           The carrier gas flow rate must be known at the given pressure. It can be measured or  calculated. In our example we assume the carrier gas flow to be v(column) = 1.3 ml/min.

·           We multiply this flow rate by the split ratio 1:50 to get the flow rate through the split vent: v(split) = 50 * 1,3 = 65 ml/min.

·           The bubble flow meter is then connected to the split vent

·           We now measure the gas flow several times while turning the split vent valve until the flow rate is near the desired value of 65 ml/min. The absolute value of the split vent flow rate is not important. It’s rather the constancy between measurements that matters.

 

 

 

Maintaining the injector

 

Changing the liner

A liner is a glass tubing inside the injector. After an extended period of operation this part can be contaminated or plugged. It should than be cleaned or exchanged. Liners are expendable items. It is not bad idea to keep one or two handy as spare parts.

·           Turn off power, pull mains plug and close all gas valves at the pressure gas cylinders.

·           Unscrew the heatsink from the top oft he injector.

·           Remove septum and pressure plate from the heat sink.

·           Pull out the liner with a suitable tool e.g. a small screwdriver.

·           Before mounting the liner its outer surface should be carefully cleaned.

·           Insert the glass tube with its indentations directing upwards into the opening of the injector. The upper end of the liner should be positioned on the same level as the rim of the injector.

·           Put the septum and then the pressure plate on top of the injector opening. (Do not change the order!) Screw the heat sink onto the injector and fasten hand tight.

 

 

Exchanging the septum

If the septum shows signs of wear it should be replaced. Follow the directions of the previous chapter, but, of course, do not remove the liner. Durability of septa depends on injection technique and varies. Use only low bleed septa. A couple of spare septa are included.

 

Exchanging the capillary column

 

The capillary column is mounted inside the column oven with two hexagonal nuts. The ends of the column are connected to the injector (left hand side) and detector (right hand side) with ferrules and column screws. (see Fig. 36)

 

 

Removal of column

 

·           Loosen column screws at both ends with wrench 8mm and pull out the ends together with screws and ferrules. In most cases the ferrules fit tightly to the capillary.

·           Loosen two nuts M3 at the column cage and take out the column including ferrules and nuts.

·           Ferrules and column screws should be left in place if possible. If you want to remove it, firmly grab the capillary between two fingers and pull the screw.

 

 

Owing to circumstances it can make sense to cut an inch or two from the end of the column. Lay the column end on to a flat surface and scratch the capillary with a carbide or diamond cutter, then bend it symmetrically over both thumbs until it breaks. Slide the screw and the ferrule over the capillary, the conical end of the ferrule must point to the end of the column, see Fig. 37 for details.

 

 

 

Beschreibung: Beschreibung: Beschreibung: Beschreibung: PrepInstCol

Preparations when installing the capillary column

 

 

 

Connecting the column on the injector side

 

It is mandatory, to follow the measures of Fig. 36 above. To insure this, it is recommended to mark the column with a felt-tip pen as shown. The column is inserted carefully into the injector. This procedure is delicate and requires some patience und manual skill.

Tighten the column screw by hand first, than fasten with wrench 7 mm. Pull slightly with two fingers at the column to check the column for firm seating. If doing so, the column must not move.

 

Beschreibung: Beschreibung: Beschreibung: Beschreibung: http://upload.wikimedia.org/wikipedia/commons/thumb/3/38/Zeichen_101.svg/500px-Zeichen_101.svg.png
 


Important note: It is indispensable to retighten the column screws after one or two heating cycles! This is all the more important if hydrogen is in use as a carrier gas

 

 


Connecting the column on the injector side

 

Connecting the column to the detector

 

The procedure is principally the same as described in the previous paragraph. If you encounter a barrier when inserting the column, we advise to move the column slightly back and forth to facilitate its way upwards until the mark is in its final position. Regard warning above!

 

 

 

Using the bubble flow meter

 

This simple but efficient flow meter essentially consists of a graduated glass tube in which a gas flow moves up a soap film.

Prior to first use, fill the rubber ball with water and add one drop of liquid kitchen detergent. Slide the rubber ball onto the lower end of the glass tube, wetting the glass end helps.

To initiate the measuring process, squeeze the rubber ball containing the detergent solution until the level of the liquid passes the gas inlet, which leads to the formation of one or more soap films.

 

Beschreibung: Beschreibung: Beschreibung: Beschreibung: Bubble_meter_eng

Bubble flow meter

 

Now select a measurement volume between two rings on the glass tube, start a timer when the film passes the first ring, stop the timer when it passes the second ring. Calculate the flow rate from the equation:

 

Flow rate:     v  =  Volume/Time [ml/min]

 

Example: Elapsed time between two marks with a distance of 2 ml:  t = 9,6 s.

v = 2 ml / 9,6 s = 0,208 ml/s

v  = 0,208 ml/s • 60 s/min   = 12 ml/min

 

You can achieve this result much more easily by using the GC software. Simply click on “Measure gas flow” and use as directed.

 

 

 

Calculating the carrier gas flow

 

 

Capillary columns are thin tubes, for which Poiseuilles law applies. The law can be written in the form

            dV/dt = v = (R/h) × Dp            (1)       where

R = k × r4/l                               (2)

Flow rate dV/dt of a gas through a thin tube is proportional to the pressure difference  Dp”

 

The factor R/h depends on the kind of gas, its viscosity, the radius r and the length l of the tube.

The following tables show calculated values for thin tubes of 0.32 mm diameter, 25 meters length at different temperatures for the following gas types: Hydrogen, helium, nitrogen. It can be used to estimate the carrier gas flow for capillary columns. Note that this is a first-order approximation.

 

 

Helium

 

Gas flow in ml/min through column 0,32 mm/25 m     pressure p in bar, T  in °C

 

p

0,1

0,2

0,3

0,4

0,5

0,6

0,7

0,8

0,9

1

1,1

1,2

1,3

1,4

1,5

T

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

20

0,57

1,14

1,72

2,29

2,86

3,43

4,01

4,58

5,15

5,72

6,30

6,87

7,44

8,01

8,59

30

0,56

1,12

1,68

2,24

2,80

3,37

3,93

4,49

5,05

5,61

6,17

6,73

7,29

7,85

8,41

40

0,55

1,10

1,65

2,20

2,75

3,30

3,85

4,40

4,95

5,50

6,05

6,60

7,15

7,70

8,25

50

0,54

1,08

1,62

2,16

2,70

3,23

3,77

4,31

4,85

5,39

5,93

6,47

7,01

7,55

8,09

60

0,53

1,06

1,59

2,11

2,64

3,17

3,70

4,23

4,76

5,29

5,82

6,34

6,87

7,40

7,93

70

0,52

1,04

1,56

2,08

2,59

3,11

3,63

4,15

4,67

5,19

5,71

6,23

6,74

7,26

7,78

80

0,51

1,02

1,53

2,04

2,55

3,06

3,57

4,07

4,58

5,09

5,60

6,11

6,62

7,13

7,64

90

0,50

1,00

1,50

2,00

2,50

3,00

3,50

4,00

4,50

5,00

5,50

6,00

6,50

7,00

7,50

100

0,49

0,98

1,47

1,96

2,46

2,95

3,44

3,93

4,42

4,91

5,40

5,89

6,39

6,88

7,37

110

0,48

0,97

1,45

1,93

2,41

2,90

3,38

3,86

4,34

4,83

5,31

5,79

6,27

6,76

7,24

120

0,47

0,95

1,42

1,90

2,37

2,85

3,32

3,80

4,27

4,74

5,22

5,69

6,17

6,64

7,12

130

0,47

0,93

1,40

1,87

2,33

2,80

3,27

3,73

4,20

4,66

5,13

5,60

6,06

6,53

7,00

140

0,46

0,92

1,38

1,83

2,29

2,75

3,21

3,67

4,13

4,59

5,05

5,50

5,96

6,42

6,88

150

0,45

0,90

1,35

1,81

2,26

2,71

3,16

3,61

4,06

4,51

4,96

5,42

5,87

6,32

6,77

160

0,44

0,89

1,33

1,78

2,22

2,66

3,11

3,55

4,00

4,44

4,88

5,33

5,77

6,22

6,66

170

0,44

0,87

1,31

1,75

2,19

2,62

3,06

3,50

3,93

4,37

4,81

5,24

5,68

6,12

6,56

180

0,43

0,86

1,29

1,72

2,15

2,58

3,01

3,44

3,87

4,30

4,73

5,16

5,59

6,02

6,45

190

0,42

0,85

1,27

1,69

2,12

2,54

2,97

3,39

3,81

4,24

4,66

5,08

5,51

5,93

6,35

200

0,42

0,83

1,25

1,67

2,09

2,50

2,92

3,34

3,76

4,17

4,59

5,01

5,42

5,84

6,26

210

0,41

0,82

1,23

1,64

2,06

2,47

2,88

3,29

3,70

4,11

4,52

4,93

5,34

5,76

6,17

220

0,41

0,81

1,22

1,62

2,03

2,43

2,84

3,24

3,65

4,05

4,46

4,86

5,27

5,67

6,08

230

0,40

0,80

1,20

1,60

2,00

2,40

2,79

3,19

3,59

3,99

4,39

4,79

5,19

5,59

5,99

240

0,39

0,79

1,18

1,57

1,97

2,36

2,76

3,15

3,54

3,94

4,33

4,72

5,12

5,51

5,90

250

0,39

0,78

1,16

1,55

1,94

2,33

2,72

3,10

3,49

3,88

4,27

4,66

5,04

5,43

5,82

 

Hydrogen

 

Gas flow in ml/min through column 0,32 mm/25 m     pressure p in bar, T  in °C

 

p

 

0,1

0,2

0,3

0,4

0,5

0,6

0,7

0,8

0,9

1

1,1

1,2

1,3

1,4

1,5

  T

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

20

 

1,27

2,54

3,81

5,08

6,36

7,63

8,90

10,17

11,44

12,71

13,98

15,25

16,53

17,80

19,07

30

 

1,25

2,49

3,74

4,98

6,23

7,47

8,72

9,96

11,21

12,45

13,70

14,94

16,19

17,43

18,68

40

 

1,22

2,44

3,66

4,88

6,10

7,32

8,54

9,76

10,98

12,20

13,42

14,64

15,86

17,08

18,30

50

 

1,20

2,39

3,59

4,79

5,98

7,18

8,37

9,57

10,77

11,96

13,16

14,36

15,55

16,75

17,95

60

 

1,17

2,35

3,52

4,69

5,87

7,04

8,21

9,39

10,56

11,73

12,91

14,08

15,25

16,43

17,60

70

 

1,15

2,30

3,45

4,60

5,76

6,91

8,06

9,21

10,36

11,51

12,66

13,81

14,96

16,12

17,27

80

 

1,13

2,26

3,39

4,52

5,65

6,78

7,91

9,04

10,17

11,30

12,43

13,56

14,69

15,82

16,95

90

 

1,11

2,22

3,33

4,44

5,55

6,66

7,76

8,87

9,98

11,09

12,20

13,31

14,42

15,53

16,64

100

 

1,09

2,18

3,27

4,36

5,45

6,54

7,63

8,72

9,80

10,89

11,98

13,07

14,16

15,25

16,34

110

 

1,07

2,14

3,21

4,28

5,35

6,42

7,49

8,56

9,63

10,70

11,77

12,84

13,91

14,98

16,05

120

 

1,05

2,10

3,16

4,21

5,26

6,31

7,36

8,41

9,47

10,52

11,57

12,62

13,67

14,73

15,78

130

 

1,03

2,07

3,10

4,14

5,17

6,20

7,24

8,27

9,31

10,34

11,37

12,41

13,44

14,48

15,51

140

 

1,02

2,03

3,05

4,07

5,08

6,10

7,12

8,13

9,15

10,17

11,18

12,20

13,22

14,23

15,25

150

 

1,00

2,00

3,00

4,00

5,00

6,00

7,00

8,00

9,00

10,00

11,00

12,00

13,00

14,00

15,00

160

 

0,98

1,97

2,95

3,94

4,92

5,90

6,89

7,87

8,85

9,84

10,82

11,81

12,79

13,77

14,76

170

 

0,97

1,94

2,90

3,87

4,84

5,81

6,78

7,75

8,71

9,68

10,65

11,62

12,59

13,56

14,52

180

 

0,95

1,91

2,86

3,81

4,77

5,72

6,67

7,62

8,58

9,53

10,48

11,44

12,39

13,34

14,30

190

 

0,94

1,88

2,82

3,75

4,69

5,63

6,57

7,51

8,45

9,38

10,32

11,26

12,20

13,14

14,08

200

 

0,92

1,85

2,77

3,70

4,62

5,54

6,47

7,39

8,32

9,24

10,17

11,09

12,01

12,94

13,86

210

 

0,91

1,82

2,73

3,64

4,55

5,46

6,37

7,28

8,19

9,10

10,01

10,92

11,83

12,74

13,66

220

 

0,90

1,79

2,69

3,59

4,48

5,38

6,28

7,18

8,07

8,97

9,87

10,76

11,66

12,56

13,45

230

 

0,88

1,77

2,65

3,54

4,42

5,30

6,19

7,07

7,96

8,84

9,72

10,61

11,49

12,38

13,26

240

 

0,87

1,74

2,61

3,49

4,36

5,23

6,10

6,97

7,84

8,71

9,58

10,46

11,33

12,20

13,07

250

 

0,86

1,72

2,58

3,44

4,30

5,15

6,01

6,87

7,73

8,59

9,45

10,31

11,17

12,03

12,89

 

 

 

Nitrogen

 

Gas flow in ml/min through column 0,32 mm/25 m     pressure p in bar, T  in °C

 

p

 

0,1

0,2

0,3

0,4

0,5

0,6

0,7

0,8

0,9

1

1,1

1,2

1,3

1,4

1,5

T

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

20

 

0,63

1,27

1,90

2,54

3,17

3,80

4,44

5,07

5,70

6,34

6,97

7,61

8,24

8,87

9,51

30

 

0,62

1,24

1,86

2,48

3,10

3,72

4,34

4,96

5,58

6,20

6,82

7,45

8,07

8,69

9,31

40

 

0,61

1,22

1,82

2,43

3,04

3,65

4,25

4,86

5,47

6,08

6,68

7,29

7,90

8,51

9,11

50

 

0,60

1,19

1,79

2,38

2,98

3,57

4,17

4,76

5,36

5,95

6,55

7,14

7,74

8,33

8,93

60

 

0,58

1,17

1,75

2,33

2,92

3,50

4,08

4,67

5,25

5,83

6,42

7,00

7,58

8,17

8,75

70

 

0,57

1,14

1,72

2,29

2,86

3,43

4,00

4,58

5,15

5,72

6,29

6,86

7,44

8,01

8,58

80

 

0,56

1,12

1,68

2,24

2,80

3,37

3,93

4,49

5,05

5,61

6,17

6,73

7,29

7,85

8,41

90

 

0,55

1,10

1,65

2,20

2,75

3,30

3,85

4,40

4,95

5,50

6,05

6,61

7,16

7,71

8,26

100

 

0,54

1,08

1,62

2,16

2,70

3,24

3,78

4,32

4,86

5,40

5,94

6,48

7,02

7,56

8,10

110

 

0,53

1,06

1,59

2,12

2,65

3,18

3,71

4,24

4,77

5,30

5,84

6,37

6,90

7,43

7,96

120

 

0,52

1,04

1,56

2,08

2,61

3,13

3,65

4,17

4,69

5,21

5,73

6,25

6,77

7,29

7,82

130

 

0,51

1,02

1,54

2,05

2,56

3,07

3,58

4,10

4,61

5,12

5,63

6,14

6,66

7,17

7,68

140

 

0,50

1,01

1,51

2,01

2,52

3,02

3,52

4,03

4,53

5,03

5,53

6,04

6,54

7,04

7,55

150

 

0,49

0,99

1,48

1,98

2,47

2,97

3,46

3,96

4,45

4,95

5,44

5,94

6,43

6,92

7,42

160

 

0,49

0,97

1,46

1,95

2,43

2,92

3,40

3,89

4,38

4,86

5,35

5,84

6,32

6,81

7,30

170

 

0,48

0,96

1,44

1,91

2,39

2,87

3,35

3,83

4,31

4,78

5,26

5,74

6,22

6,70

7,18

180

 

0,47

0,94

1,41

1,88

2,35

2,82

3,30

3,77

4,24

4,71

5,18

5,65

6,12

6,59

7,06

190

 

0,46

0,93

1,39

1,85

2,32

2,78

3,24

3,71

4,17

4,63

5,10

5,56

6,02

6,49

6,95

200

 

0,46

0,91

1,37

1,82

2,28

2,74

3,19

3,65

4,10

4,56

5,02

5,47

5,93

6,39

6,84

210

 

0,45

0,90

1,35

1,80

2,25

2,69

3,14

3,59

4,04

4,49

4,94

5,39

5,84

6,29

6,74

220

 

0,44

0,88

1,33

1,77

2,21

2,65

3,10

3,54

3,98

4,42

4,87

5,31

5,75

6,19

6,63

230

 

0,44

0,87

1,31

1,74

2,18

2,61

3,05

3,49

3,92

4,36

4,79

5,23

5,66

6,10

6,54

240

 

0,43

0,86

1,29

1,72

2,15

2,58

3,01

3,43

3,86

4,29

4,72

5,15

5,58

6,01

6,44

250

 

0,42

0,85

1,27

1,69

2,12

2,54

2,96

3,39

3,81

4,23

4,65

5,08

5,50

5,92

6,35