Residual Solvents calculation in GC

1.0 OBJECTIVE

To lay down the procedure for the Residual Solvents calculation in GC

2.0 SCOPE

This SOP is applicable to Residual Solvents calculation in GC

3.0 BACKGROUND

NIL

4.0 RESPONSIBILITY

4.1 QC-Chemist

4.2 Head-QC

5.0 PROCEDURE

5.1 For this i have taken residual solvents(Ethanol, IPA, Acetonitrile, Ethyl acetate, Toluene, Acetic acid) in the memantine Hydrochloride.

5.2 Chromatographic Conditions:

Instrument is Agilent 6890 N, Column AT-624, 30x 0.53x 3 microns, injector Temperature is 140 degrees, split is 1:5, Detector Temerature 260 degrees(FID), Carrier gas is helium, Column flow is 2.8 PSI, Load is 1 microleter, diluent is N,N dimethyl acetamide and Column is programmed in the following way

Rate(degree/min)	Temperature(degrees)	Hold Time(Min)
--	40	10
6	130	5
35	240	11

5.3 Sample preparation: 200 mg of sample in 10 ml, dissolve, dilute to volume with diluent(20 mg/ml).

5.4 Standard Preparation:

Solution -I: Transfer 127 microliters of Ethanol, 127 microliters of IPA, 11 microliters of Acetonitrile, 111 microliters of Ethyl acetate, 21 microliters of Toluene, 95 microliters of Acetic acid in 10 ml volumetric flask dilute with diluent.

Solution-II: transfer 0.1 ml of solution-I into 10 ml Volumetric flask. This solution gives 5000 ppm of ethanol, 5000 PPM of IPA, 410 PPM of ACN, 5000 PPM of ethyl Acetate, 890 PPM of Toluene, and 5000 PPM of acetic acid with respect to 20mg/ml of sample preparation.

5.5 Calculate each solvent with following the formula

B1 is area of solvent in the blank

5.6 Typical chromatograms for Standard and Sample solution:

Standard Solution Chromatogram

Sample solution Chromatograms

5.7 Let us start the calculation

Standard Areas of 2 injections(After subtracting from Blank)

STD	Ethanol	IPA	Acetonitrile	Ethyl acetate	Toluene	Acetic acid
	169889	186930	22551	149725	75567	77700
	170012	185890	22689	146678	73212	76890
sum	339901	372820	45240	296403	148779	154590
Average	169950.5	186410	22620	148201.5	74389.5	77295

* Note: I am taken only two injections for calculation

Samples area of two injections (After subtracting from Blank)

Sample	Ethanol	IPA	Acetonitrile	Ethyl acetate	Toluene	Acetic acid
	1866	23788	5733	0	1526	0
	1922	22674	5660	0	1634	0
sum	3788	46462	11393	0	3160	0
Average	1894	23231	5696.5	0	1580	0

5.8 Solvent densities:

Solvent	Specific gravity
Pentane	0.626
Petroleum ether	0.656
Hexane	0.659
Heptane	0.684
Diethyl amine	0.707
Diethyl ether	0.713
Triethyl amine	0.728
Tert-butyl methyl ether	0.741
Cyclohexane	0.779
Tert-butyl alcohol	0.781
Isopropanol	0.785
Acetonitrile	0.786
Ethanol	0.789
Acetone	0.790
Methanol	0.791
Methyl isobutyl ketone	0.798
Isobutyl alcohol	0.802
1-Propanol	0.803
Methyl ethyl ketone	0.805
2-Butanol	0.808
Isoamyl alcohol	0.809
1-Butanol	0.810
Diethyl ketone	0.814
1-Octanol	0.826
p-Xylene	0.861
m-Xylene	0.864
Toluene	0.867
Dimethoxyethane	0.868
Benzene	0.879
Butyl acetate	0.882
1-Chlorobutane	0.886
Tetrahydrofuran	0.889
Ethyl acetate	0.895
o-Xylene	0.897
Hexamethylphosphorus triamide	0.898
2-Ethoxyethyl ether	0.909
N,N-Dimethylacetamide	0.937
Diethylene glycol dimethyl ether	0.943
N,N-Dimethylformamide	0.944
2-Methoxyethanol	0.965
Pyridine	0.982
Propanoic acid	0.993
Water	1.000
2-Methoxyethyl acetate	1.009
Benzonitrile	1.01
1-Methyl-2-pyrrolidinone	1.028
Hexamethylphosphoramide	1.03
1,4-Dioxane	1.033
Acetic acid	1.049
Acetic anhydride	1.08
Dimethyl sulfoxide	1.092
Chlorobenzene	1.1066
Deuterium oxide	1.107
Ethylene glycol	1.115
Diethylene glycol	1.118
Propylene carbonate	1.21
Formic acid	1.22
1,2-Dichloroethane	1.245
Glycerin	1.261
Carbon disulfide	1.263
1,2-Dichlorobenzene	1.306
Methylene chloride	1.325
Nitromethane	1.382
2,2,2-Trifluoroethanol	1.393
Chloroform	1.498
1,1,2-Trichlorotrifluoroethane	1.575
Carbon tetrachloride	1.594
Tetrachloroethylene	1.623