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USP ON MOBILE PHASE
The USP suggests that, in order to make their assays work, one is allowed to adjust the mobile phase by 2% absolute or 30% relative, which ever is larger. DECREASING OF PEAK AREA Possible reason can be: 1. When punctering the vail septum a small hole is made and the sample simply evaporates between injections. 2. Sample decomposition. Your sample may not be stable at the temperatur which the sample is stored in the autosample and therefore you get lower and lower peak height on following runs. 3. ACETIC ACID BY GAS CHROMATOGRAPHY Thank you, Peter. My temp programme is: 40°C for 10 min, then raise to 130°C at a rate of 6°C/min, hold at 130°C for 5 min, then raise to 240°C at a rate of 35°C/min, hold at 240°C for 11 min. Ret time of acetic acid is around 22 min. The extraction of acetic acid would be the best solution I AMMONIUM ACETATE BEFFER AS A SOVENT OF MOBILE PHASE Ammonium acetate would not be my first choice at pH 6.7. Acetate has a pKa of 4.8, and ammonia has a pKa of 9.2. That said, I would not expect ammonium acetate to precipitate, but I would expect it to make a nice nutrient for microorganisms. You should be able to prevent bugs from growing (or at least slow them down) by adding 5 - 10% organic solvent (e.g., methanol) and by preparing fresh TROUBLESHOOTING CORONA (CAD) DETECTOR We have Mobile phases of 0.1% TFA in water and 0.1% TFA in Acetonitrile with a starting point of 5% Organic ramping to 100% over8 min. Don't think
5973 (GCMS) TROUBLESHOOTING Dario Miranda | Senior Service Engineer 619.690.7300 619.607.7183 6259 Progressive Ave Suite 300, San Diego CA 92154 HOT WATER WILL DAMAGE WATERS HPLC? The senior technician in my lab suggest us to prime/purge the HPLC system with about 50 mL of hot water (70 degree C), to remove any possible salt precipitate in the tubing, prior to the start of analysis. We have followed this recommendation for about 6 months, our HPLC are working fine. Last month, when the engineer from Watersvisited our
FRUSTRATING REPRODUCIBILITY ISSUES I have tried almost everything but can't seem to get it right. Apparatus: Varian GC 3380 with a 1079 injector (single-tapered liner). Temperature program: hold 0.5min at 100°C, 25°C/min, hold 6min at 280°C. Injection of 1 µl at 10µl/s. Injector at 340°C. Solvent: tert-butyl methyl ether. Split ratio 1/40. HOW DOES EMPOWER 3 IMPURITY TAB TAKE RRF INTO ACCOUNT Joined: Tue May 30, 2017 6:53 am. by ydna1977 » Fri Jul 13, 2018 5:45 am. Hi. make sure RRF are entered into 'Relative response' column and not Impurity RRF' if using calibrate quantitate functions and curve ref. Note RRF value will be the reciprocal ie RRF 0.46 for deg peak = 1/0.46 = 2.1739 in Empower. Previous topic. CHROMATOGRAPHY FORUM Sat Mar 13, 2021 2:56 pm. Data Systems / Controllers / Computers. Discussions about chromatography data systems, LIMS, controllers, computer issues and related topics. 3011.USP ON MOBILE PHASE
The USP suggests that, in order to make their assays work, one is allowed to adjust the mobile phase by 2% absolute or 30% relative, which ever is larger. DECREASING OF PEAK AREA Possible reason can be: 1. When punctering the vail septum a small hole is made and the sample simply evaporates between injections. 2. Sample decomposition. Your sample may not be stable at the temperatur which the sample is stored in the autosample and therefore you get lower and lower peak height on following runs. 3. ACETIC ACID BY GAS CHROMATOGRAPHY Thank you, Peter. My temp programme is: 40°C for 10 min, then raise to 130°C at a rate of 6°C/min, hold at 130°C for 5 min, then raise to 240°C at a rate of 35°C/min, hold at 240°C for 11 min. Ret time of acetic acid is around 22 min. The extraction of acetic acid would be the best solution I AMMONIUM ACETATE BEFFER AS A SOVENT OF MOBILE PHASE Ammonium acetate would not be my first choice at pH 6.7. Acetate has a pKa of 4.8, and ammonia has a pKa of 9.2. That said, I would not expect ammonium acetate to precipitate, but I would expect it to make a nice nutrient for microorganisms. You should be able to prevent bugs from growing (or at least slow them down) by adding 5 - 10% organic solvent (e.g., methanol) and by preparing fresh TROUBLESHOOTING CORONA (CAD) DETECTOR We have Mobile phases of 0.1% TFA in water and 0.1% TFA in Acetonitrile with a starting point of 5% Organic ramping to 100% over8 min. Don't think
5973 (GCMS) TROUBLESHOOTING Dario Miranda | Senior Service Engineer 619.690.7300 619.607.7183 6259 Progressive Ave Suite 300, San Diego CA 92154 HOT WATER WILL DAMAGE WATERS HPLC? The senior technician in my lab suggest us to prime/purge the HPLC system with about 50 mL of hot water (70 degree C), to remove any possible salt precipitate in the tubing, prior to the start of analysis. We have followed this recommendation for about 6 months, our HPLC are working fine. Last month, when the engineer from Watersvisited our
FRUSTRATING REPRODUCIBILITY ISSUES I have tried almost everything but can't seem to get it right. Apparatus: Varian GC 3380 with a 1079 injector (single-tapered liner). Temperature program: hold 0.5min at 100°C, 25°C/min, hold 6min at 280°C. Injection of 1 µl at 10µl/s. Injector at 340°C. Solvent: tert-butyl methyl ether. Split ratio 1/40. HOW DOES EMPOWER 3 IMPURITY TAB TAKE RRF INTO ACCOUNT Joined: Tue May 30, 2017 6:53 am. by ydna1977 » Fri Jul 13, 2018 5:45 am. Hi. make sure RRF are entered into 'Relative response' column and not Impurity RRF' if using calibrate quantitate functions and curve ref. Note RRF value will be the reciprocal ie RRF 0.46 for deg peak = 1/0.46 = 2.1739 in Empower. Previous topic. SURROGATE AND INTERNAL STANDARD Surrogates are organic compounds that are similar in chemical composition to the analytes of interest and spiked into environmental and batch QC samples prior to sample preparation and analysis. ATTENUATION AND FID RANGE Attenuation - reduces the analog signal to X times, at 2, 4, 8 1024. The larger division, the smaller the signal, the lower peak on the recorder. Range - sets the signal range. In the range of equal napryazhniyu detector in the range of 1 x10 x100. Important - to work correctly - radiobutton. LABSOLUTIONS ERROR 190B You can get to Services by opening the task manager. Navigate to C:\LabSolutions\Log folder. Under the "Log" folder, delete the following files, LSSLocalLog.mdb and LSSLog.mdb. Make sure NOT to delete LSSLocal.Log.mdb.template. Reboot the computer and see if LabSolutions starts, if not, proceed to the net step. LC/MS CONTAMINATION PROBLEM LC/MS contamination problem. We have been having an issue with some contamination in our Agilent 1100 LC system coupled to an API 3000 MS. For multiple compounds, the background noise was extremely high (1000 to 10000 cps) when injecting no sample (just MeOH) without a column. After replacing all parts (tubing, PVDF filter, needle, needle seat HEADSPACE VS DIRECT INJECTION For example, a 10µg (0.01µL) spike of solvent in a 250µL sample of DMAc should be reproducible at ±2% or so. Now if this 10µg was a 1% of a 1000µg sample (1mg or perhaps 1µL) the accuracy by headspace will be 0.02%. And 1µL of sample of sample in a 250µL amount of DMAc will not affect the partition of the solventfrom
IC-2100 EGC OVER VOLTAGE ERROR Eclipse Business Media Ltd, Regd in England, No. 06513189, 2 Clarendon Road, Ashford, Middlesex TW15 2QE, United Kingdom, +44 (0)161 818 7434info@sepscience.com
EMPOWER 3. AVERAGE AND RSD% OF CUSTOM FIELDS Average and RSD% of custom fields. I understand what you mean. You should be able to do this by adding the 3 CFs and dividing by 3. So if your first CF for U0101 is called U1_average (or whatever) then code a peak, real, calculated CF and the formula is (U1_Average+U2_Average+U3_Average)/3. DISPOSING OF OLD COLUMNS. Re: Disposing of old columns. 1) as filler. 2) for damaged or ostruidas renplazar chips. 3) to replace the heads of columns, in some cases it has happened that some analyst is broken a screw heads and it is necessary to replace not discarded. this if you really do not have a good budget to buy column. PEAK AREAS INCONSISTENT, BUT OFTEN FOLLOWING A PATTERN Hello again guys and girls, I am having more peak area RSD problems. If I make successive injections of the same sample, my areas will often go up a little (2-5%) each time in a definite pattern. I am trying to determine the concentration of an organophosphonate ester (bp 180-200 deg. C) in the 1mg/mL range in solutions of H2O, EtOH,DCM, and
GC-MS, HIGH NITROGEN, LOW OXYGEN LEAK???? HELP There is often a 'lag' between changing a cylinder and the problem occurring. This may be the cause of the old cylinder also giving high N2. 2.do you have an oxygen filter fitted. If you have a leak before the oxygen filetr the oxygen is removed and only the N2 left. Hopethis helps.
CHROMATOGRAPHY FORUM Separation Science offers free learning from the experts covering methods, applications, webinars, eSeminars, videos, tutorials for users of liquid chromatography, gas chromatography, mass spectrometry, sample preparation and related analytical techniques. Subscribe to our eNewsletter with daily, weekly or monthly updates: Food, Environmental ACETIC ACID BY GAS CHROMATOGRAPHY Thank you, Peter. My temp programme is: 40°C for 10 min, then raise to 130°C at a rate of 6°C/min, hold at 130°C for 5 min, then raise to 240°C at a rate of 35°C/min, hold at 240°C for 11 min. Ret time of acetic acid is around 22 min. The extraction of acetic acid would be the best solution I TROUBLESHOOTING CORONA (CAD) DETECTOR We have Mobile phases of 0.1% TFA in water and 0.1% TFA in Acetonitrile with a starting point of 5% Organic ramping to 100% over8 min. Don't think
5973 (GCMS) TROUBLESHOOTING Dario Miranda | Senior Service Engineer 619.690.7300 619.607.7183 6259 Progressive Ave Suite 300, San Diego CA 92154 HOT WATER WILL DAMAGE WATERS HPLC? The senior technician in my lab suggest us to prime/purge the HPLC system with about 50 mL of hot water (70 degree C), to remove any possible salt precipitate in the tubing, prior to the start of analysis. We have followed this recommendation for about 6 months, our HPLC are working fine. Last month, when the engineer from Watersvisited our
USE OF GLACIAL ACETIC ACID IN MOBILE PHASEHPLC MOBILE PHASE SOLVENTHPLC MOBILE PHASE STABILITYNORMAL PHASE HPLC This paper discusses the use of acetic acid as just another organic solvent for eluting proteins from reversed-phase columns. PolyLC Inc. (410) 992-5400. aalpert@polylc.com. Re: Use of Glacial Acetic Acid in Mobile Phase. adam. Posts: 363. Joined: Wed Feb 02, 2005 9:34 pm. by adam » Mon Sep 08, 2014 6:11 pm. FRUSTRATING REPRODUCIBILITY ISSUES I have tried almost everything but can't seem to get it right. Apparatus: Varian GC 3380 with a 1079 injector (single-tapered liner). Temperature program: hold 0.5min at 100°C, 25°C/min, hold 6min at 280°C. Injection of 1 µl at 10µl/s. Injector at 340°C. Solvent: tert-butyl methyl ether. Split ratio 1/40. PEAK AREAS INCONSISTENT, BUT OFTEN FOLLOWING A PATTERN Hello again guys and girls, I am having more peak area RSD problems. If I make successive injections of the same sample, my areas will often go up a little (2-5%) each time in a definite pattern. I am trying to determine the concentration of an organophosphonate ester (bp 180-200 deg. C) in the 1mg/mL range in solutions of H2O, EtOH,DCM, and
CLEAN UP OF GC/MS AFTER PHENYLBORONIC ACID DERIVATIVE Re: clean up of GC/MS after phenylboronic acid derivative. I use phenylboronic acid to quantitate 3-monocloropropane diol or 3-mcpd. It is recommended to keep the inlet at 180 deg C and use a liner with wool on the bottom. -Cool and add 2ml hexane and a small spoon of NaCl~1-2g.
HOW DOES EMPOWER 3 IMPURITY TAB TAKE RRF INTO ACCOUNTEMPOWER POWER AMPLIFIEREMPOWER AMPLIFIERSEMPOWER RF SYSTEMS INCEMPOWER RF SYSTEMS INGLEWOOD CAEMPOWER RF AMPLIFIER Joined: Tue May 30, 2017 6:53 am. by ydna1977 » Fri Jul 13, 2018 5:45 am. Hi. make sure RRF are entered into 'Relative response' column and not Impurity RRF' if using calibrate quantitate functions and curve ref. Note RRF value will be the reciprocal ie RRF 0.46 for deg peak = 1/0.46 = 2.1739 in Empower. Previous topic. CHROMATOGRAPHY FORUM In total there are 103 users online :: 3 registered, 0 hidden and 100 guests (based on users active over the past 5 minutes) Most users ever online was 599 on Tue Sep 18, 2018 9:27 am ACETIC ACID BY GAS CHROMATOGRAPHY Thank you, Peter. My temp programme is: 40°C for 10 min, then raise to 130°C at a rate of 6°C/min, hold at 130°C for 5 min, then raise to 240°C at a rate of 35°C/min, hold at 240°C for 11 min. Ret time of acetic acid is around 22 min. TROUBLESHOOTING CORONA (CAD) DETECTOR We have Mobile phases of 0.1% TFA in water and 0.1% TFA in Acetonitrile with a starting point of 5% Organic ramping to 100% over8 min. Don't think
5973 (GCMS) TROUBLESHOOTING Dario Miranda | Senior Service Engineer 619.690.7300 619.607.7183 6259 Progressive Ave Suite 300, San Diego CA 92154 USE OF GLACIAL ACETIC ACID IN MOBILE PHASEHPLC MOBILE PHASE SOLVENTHPLC MOBILE PHASE STABILITYNORMAL PHASE HPLC Hey All I have come across a few methods recently that use Glacial Acetic Acid as the mobile phase additive. So I am curious to poll the forum: Do you see any situation where glacial acetic acid has a particular benefit over other acids. FRUSTRATING REPRODUCIBILITY ISSUES Welcome to the forum. Although the peak areas are quite variable the ratios of areas on each chromatogram are probably not too bad - allthe peaks
HOT WATER WILL DAMAGE WATERS HPLC? Dear all, The senior technician in my lab suggest us to prime/purge the HPLC system with about 50 mL of hot water (70 degree C), to removeany possible salt
PEAK AREAS INCONSISTENT, BUT OFTEN FOLLOWING A PATTERN Hello again guys and girls, I am having more peak area RSD problems. If I make successive injections of the same sample, my areas will often go up a little (2-5%) each time in a definite pattern. CLEAN UP OF GC/MS AFTER PHENYLBORONIC ACID DERIVATIVE Good day - new user here. I recently implemented a good procedure for ethylene glycol quantitation out of biologicals. The method uses phenylboronic acid as the derivative, and analysis of 20uL of acetone containing the analyte via a headspace HOW DOES EMPOWER 3 IMPURITY TAB TAKE RRF INTO ACCOUNTEMPOWER POWER AMPLIFIEREMPOWER AMPLIFIERSEMPOWER RF SYSTEMS INCEMPOWER RF SYSTEMS INGLEWOOD CAEMPOWER RF AMPLIFIER EmpowersBane wrote: I have a related substances method which is a simple (Area of impurity, both known and unknown, divided by area of active*100). Im trying to use Empower 3 impurity tab and im picking "% Area against Main component" as my impurity response but how does it take into account varying RRF factors of your known impurities? ACETIC ACID BY GAS CHROMATOGRAPHY Thank you, Peter. My temp programme is: 40°C for 10 min, then raise to 130°C at a rate of 6°C/min, hold at 130°C for 5 min, then raise to 240°C at a rate of 35°C/min, hold at 240°C for 11 min. Ret time of acetic acid is around 22 min. The extraction of acetic acid would be the best solution I TAILING AND SYMMETRY The USP tailing factor is widely accepted and differs from other asymmetry calculations in that it uses the peak width at 5% of peak height divided by 2x the front width at 5%. Asymmetry is commonly calculated as the ratio of back to front width at a specified % of peak height, normally at 10%. If anyone is aware of a referencediscussing the
SEPARATION OF DIASTEREOMERS If you don't have any chiral preparative column, you should start from normal phase column (silica, cyano) and non-polar mobile phase, for diasteromers separation, silica column sometimes gives good resolution. Diasteromers are usually not possible to separate by changing gradient or buffer (as you may have noticed). TRANSFER LINE TEMPERATURE SETTING bugteller, Remember, too, that the transfer line is at vacuum whereas the front of the column is at pressure. So compounds are going to stay volatile in the last third at temperatures considerably lower than in the first third. Even so, I would typically, as a rule of thumb, set the transfer line temp. at the same or +10 to the oven ramp max temp. DECREASING OF PEAK AREA Evaporation of solvent between replicate injections usually leads to larger areas, not smaller areas. Detectors tend to show lower responses as lamps age, but not over the course of several consecutiveinjections.
NEGATIVE PEAKS WITH ESI-MS This means the signal goes down rather than up. It can happen even when the analyte doesn't itself make a signal at all. I'm not sure if that was the problem, but one thing I did that really improved the signal was used 0.1% acetic acid for my ACN/H20 reverse phase LC-MS. Adding the acid really improved the signal. DWELL TIME, CYCLES IN LC-MS/MS I am willing to give you my answer for your question. As to 12 data points per peak, we need to set up the dwell time for each ion (transition) as follows: - the number of cycles per second: 12 : 2.5 = 4.8 cycles/second. - cycle time for 8 components : 1 : 4.8 = 0.208 s =208 ms.
DISPOSING OF OLD COLUMNS. Re: Disposing of old columns. 1) as filler. 2) for damaged or ostruidas renplazar chips. 3) to replace the heads of columns, in some cases it has happened that some analyst is broken a screw heads and it is necessary to replace not discarded. this if you really do not have a good budget to buy column. PROBLEMS WITH LOW LEVEL AMINES BY GC-FID The problem is almost certainly the activity of amines. We found that they would even stick to metal and glass surfaces (ie syringe, serum vials) while still in solution, decreasing the sensitivity, especially at low concentrations. Do whatever you can to deactivate your systemand hope for
GC/FID VS GC/MS
The same setup can be used with FID detection also, but normally with that the pesticides and herbicides are detected with the ECD instead of the FID because it is much more sensitive to the halogenated compounds. Look up methods EPA8015 for compound lists for FID, method EPA8260 for volatiles and method EPA8270 for semivolatiles by GC/MSand
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