Analytical Chemistry Lab

Unit Description

image004Our laboratory is an analytical unit, which provides Elemental Analysis and LCMS Analysis service for universities, chemical and pharmaceutical companies, research and industrial foundations. We perform the following evaluations:  analysis of C, H, N and O, the halogens: Cl,Br,I,F  and S,P, all in a broad spectrum of samples, (for example, synthesized organic compounds, natural products, coal and coal derived materials, pharmaceutical, industrial samples and others), High resolution mass determination, detection and separation in a wide range of polar masses such as: small molecules, proteins, peptides and oligonucleotides.

Sample submission

Sample submission:

You need to submit your sample in a small vial that is clearly labeled with a sample code and complete an "Elemental Analysis Request Form" or (and) the “MS Request Form"

Your sample code should consist of your initials and a number that refers to an individual sample.

 

 

Request Form for Elemental analysis Determination: Elemental Analysis form

Request Form for MS Determination: MS form.

For non-HUJI clients, please complete the Payment Form: Order

 

 

Please provide as much information as possible about your sample, and what element you wish to determine. Give the formula and draw the structure or at least an indication. Deduce your %CHN, O, S, F, Cl, Br, I, and P content. It is essential that you provide your name, phone number, e-mail address, your advisor's or company name, and purchase order or account number for billing purposes.

You should provide a bare minimum of 5 milligrams for CHN analysis. You will need to provide an additional amount if you require further analysis in addition to CHN. In cases where you have a very small amount of sample, it is possible to do one CHN run with only 1 mg.

Analysis duration:

CHN and MS results are normally completed within 3 working days, but this can vary depending upon sample load and instrument problems.

Halogens, S and P analysis are usually finished within 5 working days.

You can ask for urgent analysis, at an additional cost.

Results

Results can be picked up at the laboratory or sent to you via e-mail or regular mail.

Contacts

Contact:

For further information please contact the lab team:

Lab E-mail: micro.chem@mail.huji.ac.il

Lab manager: Dr. Carina Hazan E-mail: carinah@savion.huji.ac.il

Rachel Benzicry E-mail: rachelbe@savion.huji.ac.il

 

Tel: (972) 2-6585606

Fax: (972) 2-6584934

Address:

Analytical Chemistry Lab

Institute of Chemistry
The Hebrew University of Jerusalem
Los Angeles building (80), room 114
Edmond Safra Campus, Givat Ram, Jerusalem, 9190401, Israel

(driving directions to the Los angeles building)

Elemental analysis

Elemental analysis of C, H, N and O, the halogens: Cl, Br, I, F and S, P, all in a broad spectrum of samples: synthesized organic compounds, natural products, coal and coal derived materials, pharmaceutical, industrial samples and others.

Decomposition of organic samples

Decomposition of organic samples is done using the oxygen-flask combustion method (Schoniger application) or using the Anton Paar Microwave Induced Oxigen Combustion (MIC) for the and subsequent potentiometric titration by the 835 Titrando Metrohm  Titroprocessor and by Ion chromatography analysis  using a Dionex IC system.

 

Oxygen-Flask Combustion

oxygen-flask_combustion

MIC

mic

Accuracy

CHN weight percentages are accurate and reproducible to within ± 0.3%, for a very pure sample. Halogens, S and P weight percentage are accurate and reproducible to within ± 0.5%.

 

Microbalance

microbalance

 

Accurate weighing of samples is a prerequisite for organic elemental analysis since results are presented on a weight percent basis. A microbalance is an instrument capable of making precise measurements of weight of objects of relatively small mass: of the order of a million parts of a gram.

 

 

Determination of C, H, N and O

Determination of C, H, N and O is performed using the Thermo Flash 2000 CHN-O Elemental Analyzer. It uses a simultaneous flash combustion method (950-10600C) for CHN and pyrolysis of oxygen to convert the sample elements to simple gases. The system uses a steady-state, wave front chromatographic approach to separate the controlled gases. They are detected as a function of their thermal conductivity. The analyzer uses a globally-recognized technique that is endorsed by official organizations worldwide. High speed microprocessor control, solid-state components and built-in diagnostics, provide assurance of performance fast, reliable, and accurate results for carbon, hydrogen, nitrogen, and oxygen detection.

CHN-O Elemental Analyzer

chn-o_elemental_analyzer

Determination of halogens

Determination of halogens is done using the oxygen-flask combustion method or using the Anton Paar Microwave Induced Oxigen Combustion (MIC) for the decomposition of organic samples and subsequent potentiometric titration by the 835 Titrando Metrohm Titroprocessor and by Ion chromatography analysis using a Dionex IC system.

835 Titrando

835 Titrando

Ion chromatography

Ion Chromatography

Determination of S

Determination of sulfur is done via oxygen-flask combustion method or using the Anton Paar Microwave Induced Oxigen Combustion (MIC) for the decomposition of organic samples and subsequent gravimetric titration and by Ion chromatography analysis using a Dionex IC system.

835 Titrando

835 Titrando

Ion chromatography

Ion Chromatography

Determination of phosphorus

Determination of phosphorus is done using wet decomposition of organic samples followed by spectrophotometric detection or via oxygen-flask combustion method or using the Anton Paar Microwave Induced Oxigen Combustion (MIC) for the decomposition of organic samples and subsequent by Ion chromatography analysis using a Dionex IC system.

Ion Chromatography

Ion Chromatography

 

Water Determination

Water Determination by Karl Fischer is done using 835 Titrando System consisting of a volumetric Karl Fischer titrator with built-in buret drive for volumetric Karl Fischer titrations.

Karl Fischer

Karl Fischer

MS facilities

High resolution mass determination, detection and separation in a wide range of polar masses such as: small molecules, proteins, peptides and oligonucleotides

Mass determination and separation by LCMS/MS

High Resolution Mass determination, separation, qualitative and quantitative analysis by liquid chromatography Mass spectroscopy LC(UV)MS/MS using Agilent 6520 QTOF analyzer. High-resolution LCMS/MS Quadruple Time of Flight is an identification tool which allows distinguishing peaks separated by only small m/z values and provides excellent mass accuracy < 2ppm for MS and < 4 ppm for MS/MS also allows selective detection of desired compounds in the presence of interferences. Liquid Chromatography Mass Spectrometry enables chromatographic separation, identification and quantification of compounds in a wide range of masses (50-20000). Ionization of the samples occurs in Dual Electro Spray Ionization source which is suitable for compounds that can have a charge induced and for multiply charged compounds such as: proteins, peptides, oligonucleotides. The samples for this analyzer have to be soluble in polar well vaporizable solvents.

Q-TOF LC/MS

Q-TOF LC/MS

Mass determination and separation by GCMS

Mass Determination by Gas Chromatography/Mass Selective Detector (GC/MSD) and Qualitative analysis using Agilent 5977B Series GC/MSD:  The 5977B High Efficiency Source (HES) GC/MSD is the most trusted single-quadrupole GC/MS system providing lowest Instrument Detection Limit (IDL) as low as 1.5 fg IDL and best S/N.  The ultra-efficient EI source maximizes the number of ions that are created and transferred out of the source body and into the quadrupole analyzer.

The solvents used for this GC/MSD should be non-polar vaporable solvents. The mass detection is up to m/z=600.

GCMS