Shimadzu GC 2010 (manual injection)

10 posts / 0 new
Last post
nomar
nomar's picture
Shimadzu GC 2010 (manual injection)

I am still a beginner with limited experience on GC instruments.  However, now I will be using the GC routinely and am trying to use a Shimadzu GC 2010 (wihtout an autosampler).  It is still a new system and I have not managed to submit 1 run successfully because as soon as I manually inject the inlet pressure is altered and apparently falls out of range.  It does not vary too much (only a few kPa +or -), however as soon as this happens, an error is generated : CAR1 primary pressure is out of range and acquisition stops immediately.
Does anyone have any idea why this is happening or what I'm doing wrong?
THanks!

Dr. Analytical
Dr. Analytical's picture
Please give us some

Please give us some information about your system and operating conditions:

column - length, diameter, film thickness, stationary phase type
carrier gas - type, flow
GC Settings - temperatures and flows
Injection - volume and solvent, type (split, splitless),  are you using a syringe?

nomar
nomar's picture
Hi,

Hi,

the column specifications are as follows:

0.25um film thickness, 30m length, 0.25mm internal diameter.  The stationary phase is non-polar.

Carrier gas is helium and the column flow is 0.88mL/min but also checked with 1.00mL/min (the method is still under development). (at constant pressure of 88.7kPa but also checked with 100kPa and total flow of 15mL/min and also checked with higher flow rates).

The start-up temperature is 65 degrees for 4 mins, then it increases to 260degrees at 30 degrees/min. this temperature is held for another 4 mins.  Total run time = 14.5mins.

The solvent I'm using is n-hexane and I tried injecting 1, 2 and 3uL of solvent, however, in each case I got this error.  I've tried both split and splitless.  I'm using a 10uL Hamiltonian syringe.

I am myself still inexperienced and the system I'm using is new and is being used for the first time by myself so we're still in the process of familiarising ourselves with it.

I also found something else funny - I cannot set a particular split ratio myself, it adjusts the split ratio automatically depending on the total flow.  ALso, i tried to input a particular Pressure (given that I wanted to run at constant pressure) and a particular column flow rate and split ratio.  When i adjusted these, it calculated the  total flow automatically (something which I expected), however, this flow was usually not enough to sustain the pressure I wanted and it could never reach the specified pressure.  For it to reach the specified pressure, the total flow had to be increased and subsequently it recalculated the split ratio - i was always ending up with a higher split ratio than i wanted.

Thanks a lot!

levis_mt
levis_mt's picture
Hi,

Hi,

i have been in this field for the last 5 year and from your query i would suggest that you contact your local Shimadzu supplier. If i'm not mistaken it' s Technoline Ltd. Tel: +356 21344345. They should be able to help on this.

Hope it helps!

Dr. Analytical
Dr. Analytical's picture
The GC can control the

The GC can control the pressure, flow, and split ratio, but these values are all related, so a change in one value can cause the other values to change.  I do not know how your instrument does the control (each GC is different), so I can only make some general suggestions.

1. For a 0.25 mm column, even a 1 uL injection volume may be too much.  This is a small column with a small capacity, and the column will overload easily.  Start with split injections, using a very high split ratio (for example, 1:250 ), and then decrease the ratio until you get the error.

2. Use the slower flow rates that you discussed (less than 1 mL/min). 

Can you see the pressure on the instrument or software? Does it increase or decrease before the error occurs?

nomar
nomar's picture
Thanks for your replies.

Thanks for your replies.

@ levis mt: yes, in fact I have contacted the local supplier and they should be having a look at it next week. Thanks.

@ Dr Analytical:
1. I will follow your suggestion and try out the high split ratios, i did not try such high ratios, however i did try injecting low volumes down to 1uL and even none at all (just using the syringe to puncture the septum but without actually injecting anything).  The error occurs in either case.

2.  I will try the lower column flow rates.

3. Yes I can observe the pressure while I'm injecting, occassionally it increases but usually it decreases by around 1 kPa and it still generates the error.

Thanks for your response.

mallesh.jubburu
mallesh.jubburu's picture
HI FRIENDS I AM ALSO USING

HI FRIENDS I AM ALSO USING SHIMADZU GC-2010 SYSTEM . I FACED A NEW PROBLEM THAT MY GC SYSTEM DIDN'T COME FOR READY MODE  i.e IF THE INITIAL TEMPARATURE IS 60ºC THE TEMPARATURE STANDS AT 65 OR 63ºC AND DID NOT COME TO 60ºC. I CHECKED THAT FAN IS WORKING PROPERLY.

PLEASE ADVICE ME.

THANKS.
Mallesh.J

mohmaduns
mohmaduns's picture
 Thank you very mach

 Thank you very mach
I have same proplem with gc-ms -2010 shimadzu and solve problem by your advice

Dr. Analytical
Dr. Analytical's picture
We can not offer any advice

We can not offer any advice until we have complete information about your problem.

quy vuong
quy vuong's picture
help me

I used GC 2010 with FID detecter. My system have a fail: "card 1 primary pressure is out of range" Please help me how to fix?