Trou­ble shoo­ting
gui­de

We coll­ec­ted the most com­mon pro­blems and their pos­si­ble so­lu­ti­ons in the trou­ble shoo­ting gui­de be­low. If you are not able to find a so­lu­ti­on to your pro­blem in this gui­de, plea­se do not he­si­ta­te to cont­act us.

GENERAL
INFORMATION

Vol­ta­ge

Ge­ne­ral­ly hig­her vol­ta­ge leads to a hig­her si­gnal; ho­we­ver, this doesn’t ne­ces­s­a­ri­ly trans­la­te to a hig­her S/N. A hig­her vol­ta­ge also leads to more re­ac­ti­ve spe­ci­es for­med (N2+).
Re­com­men­ded set­tings: 1300 – 1800 V. Do not set hig­her than 2000 V.

Fre­quen­cy

Fre­quen­cy is the oscil­la­ti­on of the plas­ma tur­ning off and on, the­r­e­fo­re hig­her fre­quen­cy usual­ly in­crea­ses the amount of re­ac­ti­ve spe­ci­es which in hand usual­ly leads to a hig­her si­gnal and par­ti­al­ly hig­her S/N.
Re­com­men­ded set­tings: 15000 – 50000 Hz

With di­rect scree­ning or GC/SPME mo­du­le a re­com­men­ded start­ing point is 15000 Hz.

With the LC mo­du­le a re­com­men­ded start­ing point is 50000 Hz.

La­test me­a­su­re­ments with the LC mo­du­le and high in­ta­ke flow MS sys­tems show that hig­her fre­quen­ci­es (e.g. 50kHz) can have a be­ne­fi­ci­al ef­fect on RSDs and over­all S/N.

Note: Plea­se see pa­per of Gyr, Wolf, Franz­ke, Zen­o­bi (Me­cha­ni­stic Un­der­stan­ding Leads to In­creased Io­niza­ti­on Ef­fi­ci­en­cy and Sel­ec­ti­vi­ty in Dielec­tric Bar­ri­er Di­schar­ge Io­niza­ti­on Mass Spec­tro­me­try: A Case Stu­dy with Per­fluo­ri­na­ted Com­pounds) for more de­tails on fluo­ri­na­ted hy­dro­car­bons for ex­pl­ana­ti­on and po­ten­ti­al ex­plo­ita­ti­on of the­se ef­fects.

Phy­si­cal Pro­per­ties and Li­mi­ta­ti­ons

  • The SICRIT io­niza­ti­on source is made of me­di­cal gra­de PEEK, (gold coa­ted) cop­per and cera­mic. It has long term tem­pe­ra­tu­re sta­bi­li­ty up to 260°C, and for short pe­ri­ods the PEEK can to­le­ra­te tem­pe­ra­tures up to 320°C.
  • The source can­not to­le­ra­te high con­cen­tra­ti­ons of high­ly cor­ro­si­ve acids: Ex. HF, H2SO4, Aqua re­gia
  • The source is not re­sistant against fluo­ri­ne, chlo­ri­ne, and bro­mi­ne.
    Do not use pure THF as it will cau­se swel­ling of the Peak.

Com­pa­ti­bi­li­ty with High Flow MS

The SICRIT® source in com­bi­na­ti­on with mo­du­les (po­ten­ti­al­ly di­rect scree­ning as well) is par­ti­al­ly fa­cing pro­blems with di­rect ESI swap on in­stru­ments that have very high flow in­let ca­pil­la­ries like Ther­mo Ex­plo­ris 480 or TQ ab­so­lu­te. In com­bi­na­ti­on the SICRIT® source and mo­du­le, the SC-30 con­trol unit may shut down and re­start with er­ror Low Vol­ta­ge at HV-Out­put. To com­bat this is­sue, re­place the in­ner elec­tro­de with a lar­ger in­ner dia­me­ter (cont­act Plas­mi­on).

Ion Source &
SC-30 Con­trol Unit

Source does not lock

If the source does not lock on the ad­ap­ter make sure only a sin­gle o‑ring is in­stal­led on the ion source. So­me­ti­mes, o‑rings can get stuck on the ad­ap­ter du­ring re­m­oval of the source.

Low Si­gnal

Po­ten­ti­al Re­ason So­lu­ti­on
Source is clog­ged Clean Source: Watch Clea­ning Tu­to­ri­al vi­deo.
Core needs to be re­pla­ced Re­place Core: Watch Tu­to­ri­al Vi­deo for Core Ex­ch­an­ge.
Mo­du­le is not in­stal­led pro­per­ly Check in­stal­la­ti­on:Ope­ra­ti­ons and In­stal­la­ti­ons Ma­nu­al
Mo­du­le needs ser­vicing Cont­act Plas­mi­on sup­port team
Is­sue with the Mass Spec Cont­act MS Sup­port

Flow chart for pro­blem sol­ving in case of low si­gnal:

No Si­gnal

Po­ten­ti­al Re­ason So­lu­ti­on
Source is clog­ged Clean Source: Watch Clea­ning Tu­to­ri­al vi­deo
Core needs to be re­pla­ced Re­place Core: Watch Tu­to­ri­al Vi­deo for Core Ex­ch­an­ge
SC-30 Con­trol Unit needs ser­vicing Cont­act Plas­mi­on sup­port team
Mo­du­le needs ser­vicing Cont­act Plas­mi­on sup­port team
Set­tings on the MS are not cor­rect (e.g. tube len­se vol­ta­ge, gas flows, etc.) Check Ope­ra­ti­ons and In­stal­la­ti­ons Ma­nu­al
Is­sue with the Mass Spec Cont­act MS Sup­port

Flow chart for pro­blem sol­ving in case of no si­gnal:

Unsta­ble Si­gnal

Po­ten­ti­al Re­ason So­lu­ti­on
Core needs to be re­pla­ced Re­place Core: Watch Tu­to­ri­al Vi­deo for Core Ex­ch­an­ge
In­cor­rect In­jec­tions Make sure au­to­sam­pler in­jects re­pro­du­ci­b­ly (no bubbles, tight sy­rin­ge, etc.)
Pro­blem with cou­pling to chro­ma­to­gra­phy Check in­jec­tion port (sep­ta and li­ners) and in­jec­tion set­tings (speed, split­less time, in­jec­tions depth, etc.)

High Vol­ta­ge Er­ror

Po­ten­ti­al Re­ason So­lu­ti­on
SC-30 Con­trol is­sue is de­fect Cont­act Plas­mi­on sup­port team
Ca­ble is de­fect Cont­act Plas­mi­on sup­port team
Plas­ma core is de­fect Re­place Core: Watch Tu­to­ri­al Vi­deo for Core Ex­ch­an­ge
Ion source is de­fect Cont­act Plas­mi­on sup­port team

Flow chart for pro­blem sol­ving in case of high vol­ta­ge er­ror:

Low Vol­ta­ge at HV Out­put

Po­ten­ti­al Re­ason So­lu­ti­on
Elec­tro­nics are over­load, sys­tem shuts down and re­starts Do not vary the set va­lues in short time in­ter­vals and wait un­til the ac­tu­al va­lue re­a­ched the tar­get va­lue
Wrong set­tings Re­com­men­ded set­tings:

1. Vol­ta­ge: 1300 – 1800 V
Do not set vol­ta­ge hig­her than 2000 V

2. Fre­quen­cy: 15000 Hz – 50000 Hz

Firm­ware Up­date nee­ded

In­s­truc­tions for firm­ware up­date:

  1. Cont­act Plas­mi­on to re­cei­ve an up­dated con­fig file.
  2. To up­date the firm­ware, turn off the SC-30 con­trol box, then re­mo­ve the SD-card from the front of the box.
  3. Set the SD-card to wri­te.
  4. Re­place the files “FW_SC30_0XX.bin” and config.txt” with the new firm­ware and con­fig files.
    Note: Save the old files be­fo­re re­pla­cing.
  5. Re­start the de­vice. The LED ring should blink green du­ring the re­boot­ing pro­cess, in­di­ca­ting the firm­ware is be­ing up­dated.
  6. By scrol­ling to the sta­tus tab, the new firm­ware ver­si­on should be dis­play­ed.

GC/SPME
MODULE

No Peaks

Po­ten­ti­al Re­ason So­lu­ti­on
Bro­ken co­lumn or trans­fer co­lumn Check the co­lumn in­si­de the GC-/SPME-mo­du­le
Cold spot in GC-/SPME-mo­du­le In­crease tem­pe­ra­tu­re of GC-/SPME-mo­du­le
Re­du­ced co­lumn flow Check for le­aka­ge at press fit con­nec­tors or in­let

Peak Broa­de­ning

Po­ten­ti­al Re­ason So­lu­ti­on
Cold spot in trans­fer line
  • In­crease trans­fer line tem­pe­ra­tu­re
  • Use de­ac­ti­va­ted guard co­lumn for the trans­fer from GC to MS
Cold spot in GC-/SPME-mo­du­le
  • In­crease tem­pe­ra­tu­re of GC-/SPME-mo­du­le
  • Check if li­ner is in­ser­ted com­ple­te­ly into the mo­du­le
Re­du­ced co­lumn flow Check for le­aka­ge at press fit con­nec­tors or in­let

Bro­ken Li­ner

If the li­ner breaks du­ring in­stal­la­ti­on of the GC-SPME mo­du­le, re­place it and ad­just the moun­ting to en­su­re an ali­gned con­nec­tion bet­ween the Swa­ge­lok el­bow and the SICRIT® source.

Back­ground Is­sues

Po­ten­ti­al Re­ason So­lu­ti­on
Ex­ces­si­ve co­lumn bleed
  • Use de­ac­ti­va­ted guard co­lumn to con­nect the mass spec.
  • Make sure to stay wi­thin the re­com­men­ded tem­pe­ra­tu­re ran­ge of the re­spec­ti­ve co­lumn cho­sen. Lower tem­pe­ra­tures should re­sult in lower co­lumn bleed and re­spec­ti­ve back­ground.
Roo­mair en­te­ring the sys­tem
  • Check if the Li­ner is int­act.
  • Check if the quick fit con­nec­tors for the gas flow at the Mo­du­le are lea­king.
  • In case of a bro­ken li­ner, see abo­ve: Bro­ken Li­ner

BREATH ANALYSIS
MODULE

High Back­ground

Po­ten­ti­al Re­ason So­lu­ti­on
Hy­dro­car­bon re­si­dues in the ni­tro­gen li­nes or bot­t­les In­stall ad­di­tio­nal gas fil­ters in the ni­tro­gen line

Si­gnal Sup­pres­si­on

Po­ten­ti­al Re­ason So­lu­ti­on
In­ver­se sup­pres­si­on be­ha­viour du­ring ex­ha­la­ti­on In­stall a t‑piece in­s­tead of the el­bow and di­lute the sam­ple by a fac­tor of 1:1 up to 3:1 with pure ni­tro­gen. This should sol­ve the sup­pres­si­on ef­fect but will re­du­ce the over­all sen­si­ti­vi­ty.

LC/SFC
MODULE

In­stal­la­ti­on

If you have is­sues with moun­ting the LC-Mo­du­le onto the mo­du­le ad­ap­ter, make sure you have the moun­ting screws loo­se­ned to line up the mo­du­le per­fect­ly straight with the ad­ap­ter. If it is still not go­ing in, try slow­ly twis­ting the front part of the source with the ad­ap­ter to the left while pushing it in the LC-Mo­du­le.
Do not try to push with full force, espe­ci­al­ly if your MS has a glass in­let ca­pil­la­ry. It might break!

High Back­ground

Po­ten­ti­al Re­ason So­lu­ti­on
Con­ta­mi­na­ti­on in the LC Sys­tem Flush the LC ac­cor­ding to the ven­dor ma­nu­al
Con­ta­mi­na­ti­on in the adapter/sprayer Clean adapter/sprayer
Con­ta­mi­na­ti­on in the LC-Mo­du­le Bake out the mo­du­le 1–3 days at 500 °C un­moun­ted from the MS, ide­al­ly with gas flow run­ning th­rough the mo­du­le
Room air en­te­ring the sys­tem Check for le­aka­ge at press fit con­nec­tors of mo­du­le

Poor Peak Shape

Po­ten­ti­al Re­ason So­lu­ti­on
Peak Tail­ing Ch­an­ge pre-co­lumn and use fresh sol­vents. Ch­an­ge the co­lumn. Most of the time the­re is an is­sue with the LC co­lumn.
Peak Split­ting Check all fit­tings (espe­ci­al­ly around the co­lumn) to pre­vent dead vo­lu­me. Flush co­lumn back­wards to get rid of par­tic­les and dirt.
Peak Fron­ting Try a lower con­cen­tra­ti­on / hig­her di­lu­ti­on of the standards/samples. If pos­si­ble, try to use the same sol­vent for di­luting samples as for the mo­bi­le pha­se in the be­gin­ning of the LC run.

Poor Se­pa­ra­ti­on

Check for dead vo­lu­me in the sys­tem espe­ci­al­ly at the fit­tings around the co­lumn and at the spray­er. If the se­pa­ra­ti­on is still bad or the peaks are very broad, un­mount the spray­er from the mo­du­le and hold it over a pa­per towel or in an emp­ty bea­k­er and start the pump to check if the spray is con­ti­nuous and cen­te­red. In case of a blo­cked spray­er, clean it ac­cor­ding to the clea­ning tu­to­ri­al. If se­pa­ra­ti­on is still an is­sue, the­re might be a pro­blem with the co­lumn.

Low Sen­si­ti­vi­ty

Po­ten­ti­al Re­ason So­lu­ti­on
Spray­er blo­cked Check and clean spray­er

High Pres­su­re

Po­ten­ti­al Re­ason So­lu­ti­on
Ca­pil­la­ry co­lumn blo­cked Check and clean spray­er