Monitor EPA 524.2 Quant ions!

[anabolic1980]

Hello Fellow Chromatographers!

Anyone out there have any suggestions how to be compliant with EPA 524.2 section 9.4 that requires the the quant ions to be monitored for internal standards surrogates, etc in samples. I am using ChemStation with Enviroquant 1701AA version. Is there some feature that can be utilized to tabulate these ions within a sequence? How is everyone out there doing this? Any help is MUCH APPRECIATED! THANKS!!!

I have posted this before and lost my replies on the new server... so I am sorry if this has been seen before. Currenly I am entering manual into Excel spreadsheet so there has to be an easier way?

Thanks again!

[tlahren]

This might help. http://www.chem.agilent.com/Library/use ... -90069.PDF Start on page 56 and read through the quantitation part. This will be a little different than your 1701AA software but a lot of the basics are the same. It will tell you how to set up a quantitation with Target Ions relative to those of internal standards and surrogates. If you still have questions after this then post a reply in this section again and I (or other Chemstation experts) can try to give you more specific help. You may need to upgrade to a more recent version of MSDChemstation C,D or E. EnviroQuant has some nice features but you need to get the quantitation table/database set up first for each analyte, ISTD and SURR. You will then have the ability to look at each compound and manually integrate (if needed) using the QEDIT feature (only available in version D and E I think). In previous version you have to navigate to "Quantitate", "Edit Result." The quant report can be exported to .CSV or .TXT if needed or you can just print them off. You can also have the quant method run after each analysis during the sequence run.

Lots of options and lots to learn, but it's worth the time.

Ty

[Bigbear]

I use a custom report that Agilent helped me build. I'll see if I can post what I use, and how to use it.
It may be as effective to call the 800 number and explain your problem.

[anabolic1980]

Thanks Bigbear and Tlahren! I really appreciate the info...

I thought there had to be an easier way out there than manually entering data. I am still surprised that Enviroquant does not have that function built-in eventhough it has other EPA QC features.

As to the reference to possibly upgrade to a 'newer' version of Chemstation, I do not think its possible since this a 5971 and my IT guy told me this is the latest version that can support this model. From my experience, the 5971 is a work horse and is great and handling water with P&T, so I really do not want to get rid of it.

Bigbear is that a template you recieved from Agilent for a custom report?

Thanks again guys!

[Bigbear]

I'm trying to post a copy of what I use but as yet have had no success!

Basicly the crt file takes the calculates the average response of all the IS's and surrogates from the active cal file. It then compares the sample response to the calc average, reports the % compared to the calibration. It then prints a pass or fail statement.
Has saved me much hand calculation.

[anabolic1980]

Hey Bigbear,

Did you receieve this app from Agilent? If so, do you have a contact number for them or application number? Again, I really appreciate the info! This forum is great for help!

[Yama001]

The G1701 AA software has a scheme for generating a simple internal standard recovery report - it can be found in the continuing calibration section of the Data Analysis window.

The custom reporting modules have a great deal of capability to produce whatever you like - I have not bothered with it in years myself, but Bigbear is steering you in the right direction.

[Bigbear]

I got it from their product support staff. Call the 800 number and describe what you need.
I'm still trying to post a copy of what I use but my IT department is not helping. I could send it to you via e mail.

[mckrause]

The easiest way for you to do this is through Custom Reports. We use a series of macros to do this, but they are complex, and if you're not used to macro language programming you won't know how to troubleshoot them.

In custom reports set up a report - there is a wizard that will walk you through what you want in your report. It's set up in an Excel-like format, so if you're already using Excel you can set it up, for example, to give you the areas for each compound in your calibration file. You would then be able to copy and paste into Excel.

All of the data that the custom reports generator accesses is found in a file called Detail.xls inside the custom reports folder (inside HPChem). If you open up Detail.xls you can see the data for the last sample processed - it'll give you a means of knowing which cells to reference in the custom report. As Yama001 pointed out, it is incredibly powerful - you can make it give you just about anything you want, and you can have it print automatically as a part of your data processing run.

[Bigbear]

I hope this works.
https://docs.google.com/spreadsheet/ccc ... lRxTldMV1E

This is the link? If you are familiar with custom reports it should be eazy to modify. Sa ve it in your custom reports folder ( mine is called 524QC) , then open the edit tab and drag in your compounds etc. Looks as if the math statements did not come through.

After you get it set up you can edit your quant method to run the crt. Works great for me.

Repost if you can't get it to work and I may be able to help.

Good luck

[Bigbear]

Has anyone tried to modify the spread sheet I posted ( assuming my posting attempt worked).

[anabolic1980]

Hi Bigbear!

Sorry for the delay I was tied up on another project... anyway thanks for posting the spreadsheet.

I am somewhat new to ChemStation and the custom reporting feature is entirely new to me. I am pretty much on my own to figure this one out as nobody in our division is familar at all with ChemStation. I hope I do not sound as if I am asking "dumb" or obvious questions.

Do I have to have Excel on the same data station as the ChemStation is running? When you mention copy and paste into the template, that is from the sample data file, is this done automatically when the report feature is processed against a data file?

Again, many thanks for steering me in the right direction.

[Bigbear]

Chemstation has a "mini" version of Excel that's what custom reports uses. When you open custom reports there is a tool bar containing icons. When you click on the one just to the left of the ? it opens a menu. You find what you are looking for and drag it into the spreadsheet. For the calibration data for calculating init cal click next compound until your IS is displayed. Then in the "white" part of the window open compound information by clicking on the + sign. Scroll down to calibration responses and drag each calibrators response into the spread sheet. Repeat for the surrogates. This is where the average from calibration is established. In my report this data is outside the print area.

This makes a link from the MS data to the spreadsheet. It's tough to explain, but just mess arround with it and you will get the hang of it. I was quite intimidated with it when I started.

Try it and see if you can make it work. Keep me posted and I'll try and help. The folks at Agilent can also talk you through it if you get stuck.

[anabolic1980]

HI Bigbear:

I finally had a chance to download the template and take a look at it. The calc statements did not come through, but it gave me an idea how to setup. I have a few questions if its ok. EPA 524.2 requires the monitoring of the surrogate/internal standard quant ions from the initial cal and also from the last CCC. I understand that the surr/istd must be within 50% from intial cal and 30% from the last CCC. Got that part.

In reference to your table, you average the ISTD fluorobenzene across the cal levels to obtain the average and then use this figure to compare samples? This would be the 50% acceptance for the ISTD. Now, how do you compare samples for the surrogates from intial cal when the surrogate areas are at different amounts due to the fact a calibration table is created? What is the comparison value for the surrogates since you cant average all the levels cuz they are different amounts. I know the samples are fixed at 1 ppb so that should stay constant.

Is it correct that EPA 524.2 wants 2 sets of comparison? One from the intial cal and one from the most recent CCC?

I played around with custom reports and getting the hang of it. Its a great feature with lots of options. I now know how to set up a template to pull data from the samples and import into custom database such as the quant ions of the istd and surrogates. I can create a value to compare the initial cal values of the ISTD to the sample quant ions with a function. No problem with this.

Now, how do you take the most recent CCC and compare that to the data files? The template you have setup only compares from the intial cal. Does this mean you have to have ANOTHER database everytime you want to compare the most recent CCC since it is only valid for that individual run of samples, where the other database is on going with comparison from the intial cal.

Any help to sort out this requirement with EPA 524.2 is greatly appreciated!
THANKS!!!

[Bigbear]

The way I read the method is and surrogate areas are compared to initial calibration OR the most recent CCC. I only monitor from the init. calibration. I use 5 ppb for my IS and surrogates. I split 75:1 so I meet the 1 ng BFB on column requirement. When my areas get under 60% is when I contemplate a source cleaning.
For my setup I named the spreadsheet 524QC, and when editing the method in data analysis you can have the sheet print with the method. If you don't like that option you can open the spreadsheet custom reports when you're done running and under the file heading choose multiple file select option. In the box that opens pick your processed files and the spreadsheet will print for each file.