Monday, June 9, 2008

SIM / Sacn in 5975 MSD

General, full scan is the most common form of data collection due to the ease of setup and the availability of spectral libraries for compound confirmation.

That is to say: Signal for screening for unknowns or for structural information (CID).
SIM mode, on the other hand, offers significant improvement in sensitivity over full-scan.
SIM signal for quantification of target compounds.


How is Synchronous SIM/Scan performed? What are the benefits?

Synchronous SIM/Scan is an acquisition mode that enables collection of both SIM (Selected Ion Monitoring) data and full scan data in a single run.

The Agilent SIM/Scan mode combines the best of both SIM and full scan from a single sample injection to improve productivity.
Agilent MSD ChemStation's AutoSIM feature allows you to create a SIM method automatically from ANY existing full scan method. Once you create the SIM method you can run synchronous SIM/Scan.
The Agilent Synchronous SIM/Scan offers the following benefits:
• Confirmatory information – full scan data for library search capability.
•Maximun sensitivity - SIM data enables trace analysis.
•Automated setup conversion - The AutoSIM feature automatically processes full scan data of chemical standards into SIM acquisition parameters for use in the SIM/Scan method.

How to STORE the Brominated diphenyl ethers for GC/MS

Brominated diphenyl ethers in water, soil, sediment, and tissue by GC-MS
(Draft Method 1614 from EPA)

(1) Standard solutions—Prepare from materials of known purity and composition or purchase as solutions or mixtures with certification to their purity, concentration, and authenticity.

If the chemical purity is 98 % or greater, the weight may be used without correction to calculate the concentration of the standard. Observe the safety precautions in Section 5 and the recommendation in Section 5.1.2.

(1.1) For preparation of stock solutions from neat materials, dissolve an appropriate amount of assayed reference material in solvent. For example, weigh 1 to 2 mg of BDE 99 to three significant figures in a 10-mL ground-glass-stoppered volumetric flask and fill to the mark with nonane. After the compound is completely dissolved, transfer the solution to a clean 15-mL vial with fluoropolymer-lined cap.

(1.2) When not being used, store standard solutions in the dark at room temperature in screwcapped vials with fluoropolymer-lined caps. Place a mark on the vial at the level of the solution so that solvent loss by evaporation can be detected. Replace the solution if solvent loss has occurred.

See, VIP tip: Before store the standard solutions, replace a new fluropolymer-line cap, then will eliminate the introducing of caps-impurity for next analysis.

Work hard, think smart.

Sunday, June 8, 2008

Replacing the make-up gas adapter (GC-ECD)


Replacing the make-up gas adapter (GC-ECD)

The make-up gas adapter consists of a line from the detector pneumatics manifold that carries make-up gas to a weldment that screws into the bottom of the ECD detector.

When re-installing the make-up gas adapter, ensure the following:
• Approximately six inches of the make-up gas line should reside in the oven after installation.
• The make-up gas line should be bent into a coil that loops around the bottom of the detector weldment and make-up gas adapter.

Tip:
There are two pneumatics blocks on the EPC version of the ECD pneumatics manifold. The outside block is the anode purge gas line and the inside block is the make-up gas line.

RoHS ( European Union - 2002/95/EC & 2005/618/EC)

What is the RoHS?
The Restriction of the use of certain Hazardous substances in Electrical and Electronic Equipment.

The SIX most famous toxic components are:
Pb、Hg、Cr6+、PBB、PBDE,Cd.
{ Note: Polybrominated biphenyls (PBB) and Polybrominated diphenyl ethers (PBDE)}

The general SOPs are following.

(1) Use the the
X-ray Fluorescence (photoelectric effect) to measure the elemental composition of a sample. Also FT-IR can also be used for screening, specifically for PBB and PDBE.

(2) GC-MS for the PBB&PBDE assay:
Column: POMSi 15 -30 m, 0.25 mm, .1 um.
Temp Ramp: 110 C (hold for 5 min), increase to 200 C @ 40C/min, hold for 4.5 min, then to 325 C @ 10 C/min, hold for 15 min.
Inlet Temp: 250 C.
MS: EI full scan or selecting ion scan from 200.0amu to 960.amu @ 70 KV.
( Note from EPA8270c & ISO 17025)

(3) HPLC/Uv for the PBB&PBDE assay:
Mobile Phase : 97% MeOH and 3% Buffer(0.1509 g KH2PO4 and 0.2477 g NaHPO4 in 100ml D.I H2O) @ C18 Reverse phase column.
Run time 12 min, flow rate: 1ml/min。
Solvent: n-IPA.
Wavelength: 254 nm, 210 nm.

{From M. Riess and R. van Eldik, Journal of Chromatography A,827 (1998):65-71}

(3) Colorimeter for the Cr6+ assay. See more details from EPA 3060 A, 7196A, 7199A, 218.6, ISO 3613: 2000(E).

(4) AAS or ICP-MS for the Pb、Hg、Cd assay.
See EPA 7000.

(5) Final, use ISO 5725 for data analysis.

Done... (:>) smile