For measuring dielectric constant and loss at different frequencies and temperature using LCR meter, you have to mount your pellet between two metallic plates of the same dia as your pellet to make a capacitor. Dia of the pellet may be 5mm to 10 mm and thickness 1-2 mm. Large thickness may result in small capacitance and difficult to measure with high accuracy. You can mount a heater in the sample holder for temperature variation. Use metallic sample holder for electromagnetic shielding and create vacuum inside the sample holder to avoid moisture effect. You can put any contact not necessarily gold. The only thing is that you have to check whether you have any barrier capacitance due to poor contact or not. To check it measure capacitance on pellets of different thickness. If your measured capacitance is decreasing linearly with thickness, your contact is o.k. you do not have any capacitance due to barrier. You can go through my research profile to see some recent papers on a.c conductivity and on dielectric relaxation in glasses.

Thank you very much Dr A.Kumar for your valuable answer.

1. For the dielectric measurementы some standards specified diameter to thickness ratio as 10:1 (e.g., diameter 10 mm, thickness 1 mm). This basic rule is that the diameter must be much greater then thickness to avoid edge effects and ensure the applicability of standard formulas to calculate the dielectric parameters.

2. When using electrodes pay attention to the quality of their coating to the material surfaces and to quality of those mechanical treatment. If you are using firing or sputtering methods of coating, I think you have nothing to fear. Poorly coated electrodes can cause noise or parasitic dielectric relaxation in the dielectric responce.

3. Automation of dielectric measurements I usually implement in MS Excel using VBA. This is a very simple and quick method, but demanding of computer resources. You can download Agilent (Keysight) set of libraries "IO Libraries Suite" (latest version is 16.3), which sets up the library to work with GPIB, USB, LAN connectivity, and display devices connected to the computer. It also include sample programs for different programming languages, including for VBA. You can change them acording to your needs, if you are using a device of different manufacturer, just change the names of commands in the code of macros. About temperature measurements I can add that to change the temperature you need a temperature controller, which can also be programmable.

Dear Muhammad, what ever may be the diameter you must substitute that in the formula thats it. For contact you can coat graphite or silver paste or gold. Here we are suffering without instrument :) . Everyone has different obstacles :)

Let's say you have a new LCR meter, you want to operate it, and also confirm it is giving you a reliable reading.

Many a times we spend a lot of money buying a fancy piece of equipment, and then we tend to get worried - it is measuring reliably.

In olden days the best calibrating device was an air capacitor made by Gen Rad (General radio company).company, and one would always calibrate their LCR meter with such devices.

Make a capacitor first of all with good electrodes.

If you cant make, go to the electronics lab, and pick up a ceramic capacitor of some capacitance.

Hook it up to your LCR meter, and measure the capacitance. Do a frequency varition and study.

1) Take a p-n junction, reverse bias, it , If your LCR meter can make measurements with a dc bais, measure the junction capacitance at some frequency with varying negative dc bais. Learn about the junction characteristics.

Many manufactures give the junction capacitance values for their components.

In a way you can first verify such things and satisfy yourself that your LCR meter is just working fine. 

2) Taking a standard piece of commercial teflon (1mm) thikck, put some electrodes, measure the capacitance. Compare your calculated and measured capacitance. 

Teflon dielectric constant is well known. So you can back calculate, and verify your measurements and calculations.

Once you learn to do the above tests, most of the things will be clear to you, whether you have made the contacts properly, whether your leads and sample holders are producing reliable results and the readings are believable.

Prof. K. Sreenivas

 When you said you have precise LCR meter, 

I would like to test capcitors which suitable insulators which yield capacitance in the range of a few pico farads reliably.

Similarly the precise LCR meter should be capable of telling you about the change in the pico farad values.

and be able to measure the loss tagent factor very reliably to a great accuracy.

I found GR1615A capacitance bridge to be one of the most accurate and precise bridge which I have ever encountered in my career. Try to see its specifications on the web (if you are able to find), then you will appreciate the capability of this instrument, and will also help you to compare your your new LCR meter, and test its capability.

Remember you have paid a lot of money for buying a precise LCR meter, so I would advise to go ahead and test its capability also, and satisfy yourself as a proud owner of a nice instrument which can do wonders.

K. Sreenivas

is it possible to measure the dielectric properties of solution ?

Dear all, I have a problem: When i measure my sample using the -Keysight 16451B Dielectric material test fixture-, the measurements (i.e the impedance outputs) are larger than the impedance values when using a homemade fixture (sample sandwiched between two electrodes usually silver paste or copper electrodes) . I 'm confused which one i should believe and why there is a difference between the output from these two methods. Is there any way to make corrections.Note: My instrument is Hioki 3536im LCR

Khalil Hamam, did you perform corrections? Corrections allows to compensate for any error caused by disturbances such as stray admittances and residual impedances. All modern devices allow for automatic Open/Short/Load correction. You should refer to your device manual. However, if your homemade fixture has too long wires and they are unshielded, or have a large stray capacitance, the correction will not work.

Aleksey A. Pavelko , No did't do corrections!, How often i should do the open/short compensations?.

Khalil Hamam , every time you change fixture.

Thank you Aleksey A. Pavelko ! But why do you think that corrections will not work with homemade fixtures. Do you recommend any special treatment or setup to use instead of the Keysight 16451B , i need to take measurements as a function of temperature.

Keysight 16451B can't handle higher temperatures than 55C!.

Khalil Hamam , you misunderstood me. If you assemble the fixture carefully, the correction will work. When correcting your homemade fixture, refer to the values that the 16451B shows.

Thickness must be 1-2 mm while diameter must be between 5-10 mm and may be greater. Thick pellets may give much better results