Application

Thiocyanate and Cyanide in

wastewater
Photometric Determination as Iron(III)-thiocyanate

Materials and reagents:

Reagents
Cat. No. 103883 Iron nitrate nonahydrate for analysis
Cat. No. 100456 Nitric acid 65 % for analysis
Cat. No. 116754 Water for analysis

Instruments
Cat. No. 173016 Spectroquant® VIS Spectrophotometer Prove 100 or
Cat. No. 173017 Spectroquant® UV/VIS Spectrophotometer Prove 300 or
Cat. No. 173018 Spectroquant® UV/VIS Spectrophotometer Prove 600 or
Cat. No. 109752 Spectroquant® Photometer NOVA 60A

Materials
Cat. No. 114946 Spectroquant® rectangular cells 10 mm
Cat. No. 114944 Spectroquant® rectangular cells 50 mm
Folded filter or
Membrane filter 0.45 μm pore diameter

Measurement range:
0.05 - 10.00 mg/l SCN at cell length 50 mm and 445 nm
0.3 - 50.0 mg/l SCN at cell length 10 mm and 445 nm

Hint:
Thiocyanate causes interference when cyanide is being determined in water and waste water. This is because it
reacts as cyanide and its value is included in the total sum determined. This procedure is not disrupted by 100-
fold amounts of cyanide based on thiocyanate. Separate determination of cyanide and thiocyanate allows both
components to be determined by differential analysis.

Preparing the reagent:

Reagent 1:
Dissolve 20 g iron nitrate nonahydrate in 24.5 ml of nitric acid 65 % and make up to mark with water for analysis in
a 100-ml volumetric flask.

Sample preparation:
The sample solution must be clear; if not, filter through a folded filter or membrane filter with 0.45 μm pore diameter.

Analysis:
Mix 5.0 ml of sample solution, 0.30 ml of reagent 1. Allow to stand for 10 minutes and measure at 445 nm against
water.

Merck KGaA, 64271 Darmstadt, Germany, Tel. 2017-07-20 Page 1 of 3

+49(0)6151 72-2440
EMD Millipore Corporation, 290 Concord Road,
Billerica, MA 01821, USA, +1-978-715-4321
Application

Programming of the Spectroquant® photometers:

The parameter lists for the programming of the Spectroquant® photometers can be found below.
Due to batch-specific variations, it is recommended to check the calibration function by measuring a standard
solution. In the case of deviations, perform a recalibration of the method.

Parameter list for programming the photometers Spectroquant® Prove 100, Prove 300 and Prove 600:

Name Thiocyanate Thiocyanate

Wavelength 445 nm 445 nm
Cell 10 mm 50 mm
Citation SCN SCN
Unit mg/l mg/l
Resolution 0.1 0.01
Lower and upper limit of 0.3-50.0 0.05-10.00
the measuring range
User-defined range user defined user defined
Zero point (E0) 0.000 0.000
Slope (A1) 16.207 3.236

Parameter list for programming the photometer Spectroquant® NOVA 60A:

Method number ---- ----

Method-designation SCN SCN
Wavelength 445 nm 445 nm
Citation SCN SCN
Units mg/l mg/l
Resolution 0.1 0.01
Zero point (E0) 0.000 0.000
Slope (E/C) 0.0617 0.309
Meas. range begin 0.3 0.05
Meas. range end 50.0 10.00
Reference cell 10 mm 50 mm

Merck KGaA, 64271 Darmstadt, Germany, Tel. 2017-07-20 Page 2 of 3

+49(0)6151 72-2440
EMD Millipore Corporation, 290 Concord Road,
Billerica, MA 01821, USA, +1-978-715-4321
Application

Calculation when measuring the absorbance value using the Spectroquant® photometers without programming
the method in the memory of the instrument:

Measured absorbance Result in mg/l

of samples in A [Asample * 16.207]
Cell length 10 mm
1.000 16.2

Measured absorbance Result in mg/l

of samples in A [Asample * 3.236]
Cell length 50 mm
1.000 3.24

Ordering Information
Product Catalog No.
Prove 100 VIS Spectrophotometer 4 nm spectral bandwidth Spectroquant® 173016
Prove 300 UV/VIS spectrophotometer 4 nm spectral bandwidth Spectroquant® 173017
Prove 600 UV/VIS spectrophotometer 1,8 nm spectral bandwidth Spectroquant® 173018
Photometer NOVA 60 A Spectroquant® 109752
Iron(III) nitrate nonahydrate for analysis EMSURE® ACS,Reag. Ph Eur 103883
Nitric acid 65% for analysis EMSURE® Reag. Ph Eur,ISO 100456
Water for analysis EMSURE® 116754
Rectangular cells 10 mm Spectroquant® 114946
Rectangular cells 50 mm Spectroquant® 114944

Merck KGaA, 64271 Darmstadt, Germany, Tel. 2017-07-20 Page 3 of 3

+49(0)6151 72-2440
EMD Millipore Corporation, 290 Concord Road,
Billerica, MA 01821, USA, +1-978-715-4321