Standard Operating Procedure

(vario MACRO CHNS Analyzer)

Sample Preparation
• Aggressive chemicals, acids, alkaline solutions, solvents, explosives or materials that
can create explosive gas mixtures are explicitly forbidden.
• Brief sample chemistry must be known, which the client will provide.
• Samples (only solid sample matrix) should be well homogenized, ground and dried.
• Sampling area and sample preparation tools (tweezers, spatula, etc.) must be
contaminant free and swept with acetone.
• Use tin foils or tin boats for sample packing.
• Counterbalance tin boat or tin foil so that the balance scale shows “0.0000”.
• Weigh sample (1 mg to 1g) and note down the required information in “Sample
Weighing Log Book”.
• Add sample additive (WO3 powder) to the sample in ratio of 1:1.

• Close tin tightly above the sample with the help of tweezers and micro spatula and
shape sample into a cube and press the air out.
• Make sure that no bits of tin foil protrude from the fold.
• Place prepared samples in appropriate sample trays.

Operation of the vario MACRO

• Note down the temperature and humidity of the working area. Ambient temperature
should be between 15 – 350C while relative humidity should be 30 – 80%.
• Make sure that during operation of the equipment there will be no electric power
failure. Generator and UPS must be ready in case of any power failure.
• Only well-trained and authorized persons are allowed to work on CHNS elemental
analyzer.
• Check and note pressure from two stage regulators of oxygen and helium gas
cylinders.
• Switch on PC with screen and printer, and wait for booting procedure to be ended.
• Remove carousel.

1
• Switch on the equipment by pressing green button inside the right side front door.

• The instrument will carry out a reference run of ball valve and carousel automatically.

• Replace the carousel.

• Load software by clicking “varioEL” icon.
• Turn on operation gases
o For helium gas cylinder, set pre-pressure approximately 2.0 bar so that inlet
pressure gauge shows 1.25 bar.
o For oxygen gas cylinder, set pressure 2.5 bar.
• Open file “template” and save as with new name.
• Confirm that analysis mode is CHNS in “Mode” option.

• Set CHNS parameters by clicking “Options” → “Parameters” (See page 5 – 12 of

operation manual).
• Observe in the status field, the furnace temperatures will rise up. Approximately 45 –
60 minutes are required for heaters to reach the set temperatures.
• Perform leakage test by clicking “Options” → “Miscellaneous” → “Rough Leak
Check”.
• Position the pointer at the end sample number by clicking “Edit” option.

• Input data by clicking “Edit” → “Input” for blank, run-in and sample in following
sequence:
Sample
Sample Name Sample Description Method Amount
Weight (mg)
blank Without anything 1 glut 2 6 – 12
blank Without anything 1 blank 2
blank Without anything 1 blind 1
blank Without anything 1 glut 2 4
blank Tin boat 1 glut 2 2
blank Tin + additive 1 glut 2 2
“run-in” Tin + additive + standard 0.5 glut 2 1
“run-in” Tin + additive + standard 1.0 glut 2 1
“run-in” Tin + additive + standard 2.0 glut 2 1
“run-in” Tin + additive + standard 4.0 glut 2 1
“run-in” Tin + additive + standard 6.0 glut 2 1
“run-in” Tin + additive + standard 8.0 glut 2 1
“run-in” Tin + additive + standard 10.0 glut 2 1
“run-in” Tin + additive + standard 20 glut 2 1
“run-in” Tin + additive + standard 30 glut 2 1
“run-in” Tin + additive + standard 40 glut 2 1

2
 Sample Tin + additive + sample According to Glut 2 2
sample nature
blank Without anything 1 glut 2 6

• Save the file.

• Place the prepared samples in carousel according to sequence and note the
carousel number in “Sample Weighing Log Book”.
• Start analysis by clicking “System” → “Auto”.

• Observe peak formation by clicking “Graphic View” button.

• After completion of analysis compute daily factor by clicking “Math” → “Factor”.

• Print out results by tagging the required samples.

• Save file.

Shutdown Procedure

• For short shutdowns (during analysis or breaks for one night or 2 –3 days, turn off He
supply. O2 supply should remain open for flushing purpose. Click on “Sleep/Wake
Up” option and select the appropriate shutdown conditions (see page 6-21 of
operation manual).
• For longer shutdowns (lasting several days or weeks), cool down all heaters and wait
until the temperatures are lower than 1000C (approximately 2 hours). For this
purpose, set nominal temperature to 00C by clicking “Parameters”. Exit software
program via System – Offline option. Turn off gas supplies, vario MACRO equipment
and peripheral instruments.