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Test 1-02 Aluminium Standard test Method: Photometric determination with Eriochrome cyanine R Range: 10 mm cuvette 50 mm cuvette Method 0.01 – 1.00 mg/l Al3+ not suitable 1 0/ 21 NANOCOLOR reagent set: Aluminium (Cat. No. 918 02) Wavelength: 540 nm Interferences: Strongly acidic and buffered test samples are to be adjusted to pH 6 after addition of R3. Turbid samples have to be filtered (membrane filters 0.45 µm, Cat. No. 916 50). Total aluminium can be determined with NanOx Metal (Cat. No. 918 978) and microwave decomposition. Fluoride interferes. The following quantities of ions will not interfere: ≤ 1 mg/l Fe2+, Co2+ ≤ 5 mg/l Fe3+, Cr3+, Cd2+ ≤ 10 mg/l Cu2+, Mn2+, Ni2+, Zn2+ The method can also be applied for the analysis of sea water. Procedure: Requisite accessories: piston pipettes with disposable tips, volumetric flasks 25 ml (Cat. No. 916 61) Pour into two separate volumetric flasks: Sample Blank value 20 200 1 2 2 20 200 1 2 2 ml test sample µl (= 0.2 ml) R1, mix, add spoon R2, mix ml R3, mix ml R4, mix ml distilled water µl (= 0.2 ml) R1, mix, add spoon R2, mix ml R3, mix ml R4, mix Fill up sample and blank value to 25 ml mark with distilled water, mix again and pour into cuvettes. Clean outside of cuvettes. Reaction time: 5’00 min Measurement: Analytical quality control: Reference: NANOCOLOR ® – 03/06 Call up method 1 0/ 21 Perform measurement NANOCONTROL multistandard Drinking water (Cat. No. 925 018) German standard methods for the examination of water, waste water, and sludge (E 9 to 1989) Test 1-05 Ammonium Method: Standard test Photometric determination as indophenol Ranges: 50 mm cuvette Method 10 mm cuvette NANOCOLOR reagent set: 0.01 – 0.40 mg/l NH4-N 0.01 – 0.50 mg/l NH4+ 0.01 – 0.50 mg/l NH3 0.1 – 2.0 mg/l NH4-N 0.1 – 2.5 mg/l NH4+ 0.1 – 2.5 mg/l NH3 1 0/ 51 1 0/ 52 1 0/ 53 1 0/ 51 1 0/ 52 1 0/ 53 Ammonium (Cat. No. 918 05) Wavelength: 690 nm Interferences: Only repeatedly and thoroughly rinsed glassware should be used. The blank value must be yellow, otherwise repeat test in the same flasks after rinsing. Turbid solutions have to be filtered. Colourations and finely dispersed matter can be compensated for with a correction value. The method can also be applied for the analysis of sea water. Procedure: Requisite accessories: piston pipettes with disposable tips, volumetric flasks 25 ml (Cat. No. 916 61) Pour into two separate volumetric flasks: Sample 20 ml test sample, add 1 ml R1, mix, fill to 25 ml with dist. water, add 1 NANOFIX R2, mix Blank value 20 ml distilled water, add 1 ml R1, mix, fill to 25 ml with dist. water, add 1 NANOFIX R2, mix Pour sample and blank value into cuvettes. Clean outside of cuvettes. Reaction time: 15’00 min The reaction time is valid for temperatures between +20 °C and +25 °C of sample and reagents. At lower temperatures longer reaction times are required. Measurement: Analytical quality control: Reference: NANOCOLOR ® – 03/06 Call up method 1 0/ 5 Perform measurement NANOCONTROL multistandard Drinking water (Cat. No. 925 018) German standard methods for the examination of water, waste water and sludge (DIN 38 406-E5-1) Test 1-10 Lead Extraction method Method: Photometric determination with dithizone Ranges: 50 mm cuvette 10 mm cuvette Method NANOCOLOR reagent set: Wavelength: Interferences: Procedure: 0.005 – 0.500 mg/l Pb2+ 0.03 – 1.00 mg/l Pb2+ Lead (Cat. No. 918 10 or 918 101) 520 nm Interfering ions: Bi3+, In3+ and Tl+ (0.4 mg/l Bi3+ = 0.2 mg/l Pb2+). Other cations do not interfere below 10–100 mg/l. The test only covers Pb2+ ions. Refer to Crack Set (Cat. No. 918 08) for sample pretreatment. The pH of the lead-containing solutions has to be kept below 3 even when solutions are diluted. Otherwise lead may be lost. Phosphate ions in large concentrations inhibit the extraction. If sulphide ions are present, the test sample must be evaporated to dryness with nitric acid. The method cannot be applied for the analysis of sea water. Requisiste accessories: 4 separation funnels 100 ml (Cat. No. 916 64) Pour into two separation funnels 100 ml: Sample 1st Extraction: 11 0/ 1 11 0/ 1 50 ml test sample, add 5 drops R1, mix (if this turns blue add diluted hydrochloric acid drop-by-drop until sample turns colourless), add 1 ml R2, mix (Sample turns blue, otherwise add more R2), add 5 ml R3, mix. Add R4 in small steps while shaking until sample turns colourless. Add 20 ml org. phase and 1 level spoon R5, shake for 1 minute. After phase separation use lower layer for 2nd extraction, discard upper layer (Caution, toxic!*) Blank value 50 ml dist. water, add 5 drops R1, mix, add 1 ml R2, mix (Blank value turns blue), add 5 ml R3, mix. Add R4 in small steps while shaking until blank value turns colourless. Add 20 ml org. phase and 1 level spoon R5, shake for 1 minute. After phase separation use lower layer for 2nd extraction, discard upper layer (Caution, toxic!*) . 2nd Extraction Sample Add 20 ml dist. water. to the lower layer (org. phase) from 1st extraction, add 2 ml R2, 1 ml R3, shake 1 minute, allow to separate Blank value Add 20 ml dist. water. to the lower layer (org. phase) from 1st extraction, add 2 ml R2, 1 ml R3, shake 1 minute, allow to separate * R3 contains cyanide! Detoxication of the upper layers: add sodium hydroxide solution to pH >9, add chlorine (choride of lime, sodium hypochlorite), mix and discard. Measurement: Analytical quality control: Reference: NANOCOLOR ® – 03/06 Do not empty organic phase into drains. After phase separation filter lower layers through funnels with wadding into two cuvettes. Clean outside of cuvettes. Call up method 11 0/ Perform measurement NANOCONTROL multistandard Metals 2 (Cat. No. 925 016) German standard methods for the examination of water, waste water and sludge (E 6 to 1981) Thomas / Chamberlin, Colorimetric Chemical Analytical Methods Test 1-13 Cadmium Extraction method Method: Photometric determination with dithizone Ranges: 50 mm cuvette 10 mm cuvette Method NANOCOLOR reagent set: Wavelength Interferences: Procedure: 1st Extraction 2nd Extraction Measurement: Analytical quality control: Reference: NANOCOLOR ® – 03/06 0.002 – 0.200 mg/l Cd2+ 0.02 – 0.50 mg/l Cd2+ 1131 1131 Cadmium (Cat. No. 918 13 or 918 131) 520 nm Only dissolved Cd2+ ions are determined. Refer to NanOx Metal (Cat. No. 918 978) or Crack Set (Cat. No. 918 08) for sample pretreatment. Strongly alkaline and buffered test samples should be adjusted to pH 3 before determination. The following ions interfere: S2– (by determining less cadmium than actually present), Co2+ (brown-violet colour) – Cadmium causes a pinkish red colour. The following quantities of ions will not interfere: ≤ 10 mg/l Fe3+, Mn2+, Pb2+, Zn2+, SCN– ≤ 1 mg/l Hg2+, CN–, S2O32– ≤ 0.2 mg/l Cu2+ The method cannot be applied for the analysis of sea water. If you encounter any problems in applying this test please contact MACHEREY-NAGEL. Requisite accessories: 2 separation funnels 100 ml (Cat. No. 916 64) Pour into two separation funnels 100 ml: Sample Blank value 50 ml test sample, add 2 ml R1, mix pH must be 3.0-3.5, adjust if necessary , add 20 ml org. phase and 1 level spoon R2, shake for 1 minute, after phase separation draw off lower layer completely and discard* add 4 ml R3, mix, add 20 ml org. phase and 1 level spoon R4, shake for 1 minute allow to separate 50 ml dist. water (do not perform 1st extraction) add 4 ml R3, mix, add 20 ml org. phase and 1 level spoon R4, shake for 1 minute allow to separate * If the colour of the lower layer is no longer green, significant quantities of interfering heavy metals are present (repeat first extraction with org. phase and R2). Organic phase which is not separated interferes with the second extraction. Do not empty organic phase into drains. After phase separation discard first 2 – 3 ml of each of the lower layers, then filter lower layers through funnels with wadding into cuvettes. Clean outside of cuvettes. Call up method 1131 Perform measurement NANOCONTROL multistandard Metals 1 (Cat. No. 925 015) G. Iwantscheff: Das Dithizon und seine Anwendung in der Mikro- und Spurenanalyse, Verlag Chemie Test 1-132 Cadmium KS Extraction method Method: Photometric determination of cadmium in sludge Range: 50 mm cuvette Method 1 – 100 mg Cd / kg S 1132 NANOCOLOR reagent sets: Cadmium KS (Cat. No. 918 132) and Cadmium (Cat. No. 918 13) Wavelength: 520 nm Interferences: The following ions interfere: Co2+ (brown-violet colour) – Cadmium causes a pinkish-red colour. Procedure: Requisite accessories: 2 separation funnels 100 ml (Cat. No. 916 64) Pour into two separation funnels 100 ml: Sample Blank value Preextraction: 20 ml decomposition solution II from NANOCOLOR Sludge (Cat. No. 918 50), fill to about 50 ml with dist. water, add 2 ml R1 (from test 1-13), mix, add 20 ml chloroform and 3 measuring spoons R2, shake for 1 minute, after phase separation draw off lower layer completely and discard* – 1st Extraction: add 20 ml org. phase and 1 level spoon R2, shake for 1 minute, after phase separation draw off lower layer completely and discard* – 2nd Extraction: add 4 ml R3, mix 20 ml org. phase 1 level spoon R4 shake 1 minute allow to separate 50 4 20 1 ml dist. water, add ml R3, mix ml org. phase level spoon R4 shake 1 minute allow to separate Shake evenly. Vigorous shaking will cause an emulsion to be formed. * Organic phase which is not separated interferes with the next extraction. Do not empty organic phase into drains. After phase separation discard first 2 – 3 ml of each of the lower layers, then filter lower layers through funnels with wadding into cuvettes. Clean outside of cuvettes. Measurement: Call up method 1132 Perform measurement Reference: G. Iwantscheff: Das Dithizon und seine Anwendung in der Mikro- und Spurenanalyse, Verlag Chemie NANOCOLOR ® – 03/06 Test 1-16 Chlorine Standard test Method: Photometric determination of the free and total chlorine with N,N-diethyl-1,4-phenylene diamine (DPD) Ranges: 50 mm cuvette 10 mm cuvette Method 0.02 – 2.00 mg/l Cl2 0.1 – 10.0 mg/l Cl2 1161/2 1161/2 NANOCOLOR reagent set: Chlorine (Cat. No. 918 16) Wavelength: 540 nm Interferences: Turbidity caused by suspended matter can be removed by centrifuging the test sample. For chlorine determinations lower than 0.1 mg/l measurement must be performed against a true blank value, which consists of distilled water with R1 to R3. For values above 5 mg/l Cl 2 add 2 spoons R2. When the chlorine concentration is > 20 mg/l, the red colouring may become bleached (inferior test results). The addition of more R2 will clearly intensify the colour. The determination of free chlorine measures bromine, bromoamines, iodine and, in part, chlorine dioxide as well. Oxidising manganese compounds simulate free chlorine. Only repeatedly and thoroughly rinsed glassware should be used. Deposits of R3 will cause falsely increased values of free chlorine. The method can also be applied for the analysis of sea water. Procedure: Requisite accessories: piston pipettes with disposable tips, volumetric flasks 25 ml (Cat. No. 916 61). Pour into two separate volumetric flasks: Sample Determination of free chlorine: 20 ml test sample, add 1 ml R1, mix 1 spoon R2, mix Blank value 20 ml test sample – – Fill up sample and blank value to 25 ml mark with distilled water, mix again and pour into cuvettes. Clean outside of cuvettes. Reaction time: 0’30 min Measurement: Call up method 1161 Perform measurement Sample Determination of total chlorine: 20 1 1 5 ml test sample, add ml R1, mix, spoon R2, mix drops R3, mix Blank value 20 ml test sample – – – Fill up sample and blank value to 25 ml mark with distilled water, mix again and pour into cuvettes. Clean outside of cuvettes. Reaction time: 3’00 min Measurement: Call up method 1162 Perform measurement Please note: The total chlorine can be determined directly after the determination of the free chlorine by adding R3 to the same cuvette (mix and measure after 3 min). Combined (bound) chlorine can be determined as being the difference between total chlorine and free chlorine. Analytical quality control: NANOCONTROL Chlorine (Cat. No. 925 17) Observe enclosed instructions! Reference: German standard methods for the examination of water, waste water and sludge (DIN EN ISO 7393-1-G4-2) NANOCOLOR ® – 03/06 Test 1-163 Chlorine dioxide Method: Standard test Photometric determination of chlorine dioxide with N,N-diethyl-1,4-phenylene diamine (DPD) Range: 50 mm cuvette NANOCOLOR reagent set: Chlorine dioxide (Cat. No. 918 163) Wavelength: 540 nm Interferences: Free chlorine is not determined with this procedure and does not interfere. Method 0.04 – 4.00 mg/l ClO2 1163 The method can be applied for the analysis of sea water. Procedure: Requisite accessories: piston pipettes with disposable tips, volumetric flasks 25 ml (Cat. No. 916 61) Pour into two separate volumetric flasks: Sample 20 1 1 1 ml test sample and ml Chlorine R4, mix ml Chlorine R1, mix measuring spoon Chlorine R2, mix Blank value 20 ml dist. water and – 1 ml Chlorine R1, mix 1 measuring spoon Chlorine R2, mix Fill up sample and blank value to 25 ml mark with distilled water, mix again and pour into cuvettes. Clean outside of cuvettes. Reaction time: measure immediately Measurement: NANOCOLOR ® – 03/06 Call up method 1163 Perform measurement R5 and R6 are not needed for this determination. Test 1-164 Chlorine – Chlorine dioxide – Chlorite simultaneously Standard test Method: Photometric determination of the chlorine compounds with N,N-diethyl-1,4-phenylene diamine (DPD) Ranges: 50 mm cuvette Method NANOCOLOR reagent set: Wavelength: Interferences: Procedure: 0.02 – 2.00 mg/l Cl2 0.04 – 4.00 mg/l ClO2/ClO2– 1164 Chlorine dioxide (Cat. No. 918 163) 540 nm For a good reproducibility, we recommend uninterrupted speedy work during sampling. Prepare values A through D in parallel. Measure sample with measuring cylinder 25 ml. To avoid errors, always use the same volumetric flasks for blank and values A to D. Requisite accessories: piston pipettes with disposable tips, volumetric flasks 25 ml (Cat. No. 916 61). Pour into five separate volumetric flasks: Blank value 20 ml dist. water 1 ml Chlorine R1, mix 1 measuring spoon Chlorine R2, mix Value A – Chlorine dioxide 1 20 1 1 Measurement: ml Chlorine R4 and ml test sample, mix, ml Chlorine R1,mix measuring spoon Chlorine R2, mix 20 ml test sample, add 1 ml Chlorine R1, mix, 1 measuring spoon Chlorine R2, mix 2 tablets Chlorine R3, mix, wait 3 min Note: NANOCOLOR ® – 03/06 – 20 ml test sample, add 1 ml Chlorine R1, mix 1 measuring spoon Chlorine R2, mix Fill up values A, B and the blank value to 25 ml mark with distilled water, mix again and pour into cuvettes. Clean outside of cuvettes. Call up method 1164 measure immediately (for this test extinctions are measured) Value C – Combined chlorine Evaluation: Value B – Free chlorine Value D – Chlorite 1 ml Chlorine R5, 2 tablets Chlorine R3 and 20 ml test sample, mix, wait 3 min, add 1 ml Chlorine R6, mix, add 1 measuring spoon Chlorine R2, mix Fill up values C and D to 25 ml mark with distilled water, mix again and pour into cuvettes. Clean outside of cuvettes. Measurement of extinctions is performed as above. A x 2.07 = mg/l chlorine dioxide (ClO2) (B – A) x 1.09 = mg/l free chlorine (Cl2) (C – B) x 1.09 = mg/l combined chlorine (Cl2) [D – (4A + C)] x 0.52 = mg/l chlorite (ClO2–) Chlorite is only present if value D > (4A + C). A negative result for chlorite means that no chlorite is present. Test 1-20 Chloride Standard test Method: Photometric determination with mercury(II) thiocyanate and iron(III) nitrate Ranges: 50 mm cuvette 0.2 – 20.0 mg/l Cl– 12 0/ 1 10 mm cuvette 1 mg/l Cl– 12 0/ 1 Method – 125 NANOCOLOR reagent set: Chloride (Cat. No. 918 20) Wavelength: 470 nm Interferences: Thiocyanate, sulphide, thiosulphate, bromide and iodide all interfere since they react in the same way as chloride. A fluoride concentration in excess of 20 mg/l interferes in the chloride determination, and the concentrations read off are lower than those actually present in the test sample. The method cannot be applied for the analysis of sea water. Note: For the determination of chloride in concrete contact MACHEREY-NAGEL for special working instructions. Procedure: Requisite accessories: piston pipettes with disposable tips, volumetric flasks 25 ml (Cat. No. 916 61) Pour into two separate volumetric flasks: Sample 20 ml test sample, add 2 ml R1, mix, add 2 ml R2, mix Blank value 20 ml dist. water, add 2 ml R1, mix, add 2 ml R2, mix Fill up sample and blank value to the 25 ml mark with distilled water, mix again and pour into cuvettes. Clean outside of cuvettes. Reaction time: 1’00 min Measurement: Analytical quality control: Reference: NANOCOLOR ® – 03/06 Call up method 12 0/ Perform measurement NANOCONTROL multistandard Drinking water (Cat. No. 925 018) Thomas / Chamberlin, Colorimetric Chemical Analytical Methods. German standard methods for the examination of water, waste water and sludge (DIN EN ISO 15682) Test 1-25 Chromate Standard test Method: Photometric determination with diphenylcarbazide Ranges: 50 mm cuvette Method 10 mm cuvette 0.01 – 0.45 mg/l Cr(VI) 1251 0.01 – 1.00 mg/l CrO42– 1252 0.1 – 3.0 mg/l Cr(VI) 1251 0.1 – 6.0 mg/l CrO4 NANOCOLOR reagent set: 2– 1252 Chromate (Cat. No. 918 25) Wavelength: 540 nm Interferences: Chromium(III) ions are not determined. For the determination of total chromium refer to NanOx Metal (Cat. No. 918 978) for sample pretreatment. The following ions will not interfere: Ca, Mn(II), Ni, Zn, CN–; ≤ 100 mg/l Cu, Fe, Pb; ≤ 10 mg/l NO2–. Colourations, turbidities, and higher amounts of organic substances, oxidising and reducing agents interfere. The method can also be applied for the analysis of sea water. Note: For the determination of chromate in electroplating baths or water-soluble chromium(VI) in cement contact MACHEREY-NAGEL for special working instructions. Procedure: Requisite accessories: piston pipette with disposable tips, volumetric flasks 25 ml (Cat. No. 916 61) Pour into two separate volumetric flasks: Sample 1 level measuring spoon Chromate R1 2 ml Chromate R2, shake vigorously for 1 min; add 20 ml test sample, mix Blank value – – 20 ml test sample Fill up sample and blank value to 25 ml mark with distilled water, mix again and pour into cuvettes. Clean outside of cuvettes. Reaction time: 5’00 min Measurement: Analytical quality control: Reference: NANOCOLOR ® – 03/06 Call up method 125 Perform measurement NANOCONTROL Chromate (Cat. No. 925 24) German standard methods for the examination of water, waste water and sludge (DIN 38 405-D24) Test 1-253 total Chromium Standard test Acidic oxidation of chromium(III) to chromium(VI) and subsequent determination with diphenylcarbazide Method: Method Ranges: 50 mm cuvette 10 mm cuvette NANOCOLOR reagent sets: Wavelength: Interferences: Procedure: 0.05 – 4.50 mg/l Cr 0.5 – 30.0 mg/l Cr 1253 1253 total Chromium (Cat. No. 918 253) and Chromate (Cat. No. 918 25) or NanOx Metal (Cat. No. 918 978) and Chromate (Cat. No. 918 25) 540 nm The following ions will not interfere: Ca, Mn(II), Ni, Zn, CN –; ≤ 100 mg/l Cu, Fe, Pb; ≤ 10 mg/l NO2–. The method can also be applied for the analysis of sea water. Requisite accessories: NANOCOLOR heating block, electric air pump with glass feed tube (Cat. No. 916 55), NANOCOLOR test tubes 14 mm ID (Cat. No. 916 80), piston pipette with disposable tips, volumetric flasks 25 ml (Cat. No. 916 61) Sample a. Preparation of sample Pipette into a test tube with 14 mm ID 2.0 ml Chromium R1, add 2.0 ml test sample solution and add one glass spiral, mix. Roll a strip of paper (e. g. around a pencil) and place inside test tube (see sketch below). The paper should remain firmly positioned against the side of the test tube and protrude just above the top of the test tube. from the air pump short side NANOCOLOR ® – 03/06 Switch on heating block, set to 148 °C and 2 h 00 min, place test tube in heating block and press "START". Switch on air pump and suspend the glass feed tube in the test tube as shown in the figure. After 2 h remove test tube with the residue (first switch off air pump and remove glass feed tube from test tube). Allow test tube to cool down. Remove the strip of rolled paper from the test tube. 1 Test 1-253 total Chromium (continued) Sample b. Oxidation Carefully add 4.0 ml Chromium R2 to test tube, mix. Add 1 level spoon Chromium R3, close tube with screw cap and mix. Switch on heating block, set to 100 °C and 30 min. Place test tube in heating block. Press “START” (Attention! Heating block only works if it has cooled to below 100 °C in the meantime – safety precaution.) After 30 min remove test tube and allow to cool down. c. Determination of chromium Sample Standard test (test 1-25) Pour into a volumetric flask: 1 level measuring spoon Chromate R1 2 ml Chromate R2, shake vigorously for 1 min; Add the contents of the test tube from step b with the aid of a glass funnel. Rinse the test tube 3 times, each time with 5 ml distilled water Fill up sample to 25 ml mark with distilled water, mix again and pour into a cuvette. Clean outside of cuvette. Reaction time: 5’00 min Measurement: Call up method 1253 Perform measurement Note: Chromium (III) = total chromium – chromium(VI) = total chromium – (chromate x 0.45) Analytical quality control: NANOCOLOR ® – 03/06 NANOCONTROL multistandard Metals 1 (Cat. No. 925 015) 2 Test 1-30 Method: Ranges: NANOCOLOR reagent set: Cyanide Standard test Photometric determination with barbituric acid/pyridine 50 mm cuvette 10 mm cuvette 0.001 – 0.100 mg/l CN– 0.01 – 0.50 mg/l CN– Method 13 0/ 1 13 0/ 1 Cyanide (Cat. No. 918 30) Wavelength: 585 nm Interferences: Cyanide concentrations lower than 0.01 mg/l must be measured against a reagent blank value. Thiocyanate interferes by reacting the same way as cyanide (investigation with Thiocyanate 50 test 0-91). Only free cyanide and cyanide complexes, which can be decomposed by chlorine, are determined. When interfering substances, such as heavy metal complexes, thiocyanate, sulphide, dyes or aromatic amines are present, cyanide must be separated by distillation before determination. The method can also be applied for the analysis of sea water. Note: For the determination of readily liberated cyanide and total cyanide contact MACHEREY-NAGEL for special working instructions. Procedure: Requisite accessories: piston pipettes with disposable tips, volumetric flasks 25 ml (Cat. No. 916 61) Pour into two separate volumetric flasks: Sample 20 ml test sample, add 1 level small spoon R1, dissolve, wait 1 minute, add 1 level large spoon R2, mix thoroughly (some grains remain undissolved), add 2 ml R3, mix Blank value 20 ml test sample – – – Fill up sample and blank value to 25 ml mark with distilled water, mix thoroughly and pour into cuvettes. Clean outside of cuvettes. Reaction time: 5’00 min Measurement: Call up method 13 0/ Perform measurement Reference: German standard methods for the examination of water, waste water and sludge (DIN 38 405-D13-2-3/-D14-2) NANOCOLOR ® – 03/06 Test 1-32 Detergents (anionic surfactants) Extraction method Method: Photometric determination with methylene blue Ranges: 50 mm cuvette 10 mm cuvette Method 0.02 – 1.00 mg/l MBAS 0.1 – 5.0 mg/l MBAS 1321 1321 NANOCOLOR reagent set: Detergents anionic (Cat. No. 918 32) Wavelength: 620 nm Interferences: If the water contains cationic detergents in addition to the anionic ones, equivalent quantities are combined which escape analysis. Sulphide ions must be removed by the addition of hydrogen peroxide. In order to achieve optimum test results, it is essential that all glassware be thoroughly cleaned before use. Washing with 10% alcoholic hydrochloric acid followed by chloroform is most suitable for this purpose. The method cannot be applied for the analysis of sea water. Procedure: Requisite accessories: 4 separation funnels 100 ml (Cat. No. 916 64) Pour into two separation funnels 100 ml: Sample 1st Extraction: 50 2 1 20 Blank value ml test sample, add ml R1, mix, add ml R2, mix, add ml org. phase shake for 1 minute, allow to separate 50 2 1 20 ml dist. water, add ml R1, mix, add ml R2, mix, add ml org. phase shake for 1 minute, allow to separate Shake evenly. Vigorous shaking will cause an emulsion to be formed. Pour into two other separation funnels 100 ml: Sample 2nd Extraction: Blank value 50 ml dist. water, add 1 ml R3, mix Add lower org. phase from the 1st separation funnel, shake for 1 minute 50 ml dist. water, add 1 ml R3, mix Add lower org. phase from the 1st separation funnel, shake for 1 minute After phase separation filter each of the lower layers through funnels with wadding into cuvettes. Too much wadding produces inaccurate test results. Clean outside of cuvettes. Measurement: Call up method 132 Perform measurement Interpretation: Anionic detergents refer to dodecylbenzenesulphonic acid methyl ester. To analyse anionic detergents of known composition, the following correction is necessary: X Test result = Measured value ⋅ ---------341 X = molar mass of substance to be determined Do not empty org. phase into drains. Reference: NANOCOLOR ® – 03/06 German standard methods for the examination of water, waste water and sludge (DIN 38 409-H23-1) Test 1-34 Detergents (cationic surfactants) Extraction method Method: Photometric determination with bromophenol blue Ranges: 50 mm cuvette 10 mm cuvette Method 0.05 – 3.00 mg/l CTAB 0.2 – 5.0 mg/l CTAB 1341 1341 NANOCOLOR reagent set: Detergents cationic (Cat. No. 918 34) Wavelength: 436 nm Interferences: If the water contains anionic detergents in addition to the cationic ones, equivalent quantities are combined which escape analysis. In order to achieve optimum test results, it is essential that all glassware be thoroughly cleaned before use. The most suitable solvent is ethanol. The method cannot be applied for the analysis of sea water. Procedure: Requisite accessories: 2 separation funnels 100 ml (Cat. No. 916 64) Pour into two separation funnels 100 ml: Sample 50 2 1 20 Blank value ml test sample, add ml R1, mix, add spoon R2, dissolve, add ml org. phase, shake for 3 minutes 50 2 1 20 ml dist. water, add ml R1, mix, add spoon R2, dissolve, add ml org. phase, shake for 3 minutes After phase separation filter each of the lower layers through the funnels with wadding into cuvettes. Clean outside of cuvettes. Measurement: Call up method 134 Perform measurement Interpretation: Cationic detergents refer to N-cetyl-N,N,N-trimethylammonium bromide (CTAB). To analyse cationic detergents of known composition, the following correction is necessary: X Test result = Measured value ⋅ --------------364.5 X = molar mass of substance to be determined Do not empty org. phase into drains. Reference: NANOCOLOR ® – 03/06 German standard methods for the examination of water, waste water and sludge (H 23 until 1980) Test 1-36 Method: Iron Standard test Photometric determination with 1,10-phenanthroline Method Ranges: NANOCOLOR reagent set: 50 mm cuvette 10 mm cuvette 0.01 – 2.00 mg/l Fe 0.1 – 15.0 mg/l Fe 1361 1361 Iron (Cat. No. 918 36) Wavelength: 470 nm Interferences: Complex iron compounds are not determined by this test. Oxidising reagents interfere with the determination. The following quantities of ions will not interfere: ≤ 10 mg/l Co, Ni ≤ 25 mg/l Cu, Zn ≤ 100 mg/l PO43– The method can also be applied for the analysis of sea water. Note: Only dissolved iron and easily soluble iron compounds can be determined with this procedure. We recommend the following methods to distinguish between total iron and dissolved iron: A) determination of the dissolved iron after filtration through a membrane filter 0.45 µm (Cat. No. 916 50) B) determination of total iron after decomposition with NanOx Metal (Cat. No. 918 978) or with Crack Set (Cat. No. 918 08) Determination of iron(II) ions is performed as below, but without addition of Iron R2. [1] For the sensitive determination of iron using 50 mm cuvettes a reagent blank value (dist. water plus reagents) is required. Procedure: Requisite accessories: piston pipettes with disposable tips, volumetric flasks 25 ml (Cat. No. 916 61) Pour into two separate volumetric flasks: Sample 20 1 1 1 1 ml test sample, add ml R1, mix, add spoon R2, mix, add ml R3, mix, add ml R4, mix Blank value [1] 20 ml test sample – – – – Fill up sample and blank value to 25 ml mark with distilled water, mix again and pour into cuvettes. Clean outside of cuvettes. Reaction time: 5’00 min Measurement: Analytical quality control: Reference: NANOCOLOR ® – 03/06 Call up method 136 Perform measurement NANOCONTROL multistandard Drinking water (Cat. No. 925 018) German standard methods for the examination of water, waste water and sludge (DIN 38 406-E1-1) Test 1-39 Colour (DIN or Hazen) Method: Standard test Photometric determination of the Hazen colour (APHA Platinum-Cobalt-Chloride Standards) or the colour at different wavelengths Ranges: 50 mm cuvette Method 5 – 500 mg/l Pt (units on the Hazen colour scale) Results shown as spectral absorbance coefficient in accordance with the German Standard Methods (DIN): Colour in m–1 0.2 – 20.0 1/m (∆ λ = 10 nm) at 436 nm at 520 nm at 620 nm 1391 1392 1393 1394 Wavelengths: 436, 520 or 620 nm Interferences: Turbid solutions must first be filtered (membrane filter kit 0.45 µm, Cat. No. 916 50). Should the turbidity reading also be required as a comparison, then the difference between the test results before and after filtration can be used. Procedure: Pour directly into two separate dry cuvettes Sample Blank value test sample distilled water Measurement: Call up method 139 Perform measurement The method can be applied for the analysis of sea water. Reference: Standard Methods for the Examination of Water and Waste Water, APHA (American Public Health Association), AWWA (American Water Works Association), WEF (Water Environment Federation), 18 th Edition 1992 German standard methods for the examination of water, waste water and sludge (DIN EN ISO 7887 C1) NANOCOLOR ® – 03/06 Test 1-42 Fluoride Standard test Method: Photometric determination of fluoride with 1,8-dihydroxy-2-(4-sulfophenylazo)naphthalene-3,6-disulphonic acid (SPADNS) Range: 10 mm cuvette NANOCOLOR ® reagent set: Fluoride (Cat. No. 918 142) Wavelength: 585 nm Interferences: Only repeatedly and thoroughly rinsed glassware should be used. Sea water and waste water require a distillation. The following ions will not interfere: < 1000 mg/l Cu2+; < 500 mg/l Ca2+, Ni2+, Zn2+; < 200 mg/l Fe3+; < 100 mg/l SO42–; < 50 mg/l Cr(III); < 20 mg/l Si(IV); < 10 mg/l Cr(VI); < 5 mg/l PO43–, Cl2; < 0.1 mg/l Al3+ Requisite accessories: volumetric flasks 25 ml, piston pipettes with tips Method Procedure: Measurement: Reference: NANOCOLOR ® – 03/06 0.05 – 2.00 mg/l F– Sample Blank value 20 ml test sample, 2.0 ml R1, mix 20 ml dist. water, 2.0 ml R1, mix 1421 Fill up sample and blank value to 25 ml mark with distilled water, mix and pour into cuvettes. Clean outside of cuvettes. Reaction time: 5’00 min Call up method 142 Perform measurement Standard methods for the examination of water and wastewater (4500-F –-D) Test 1-44 Method: Hydrazine Standard test Photometric determination with 4-dimethylaminobenzaldehyde Method Ranges: NANOCOLOR reagent set: 50 mm cuvette 10 mm cuvette 0.002 – 0.250 mg/l N2H4 0.01 – 1.50 mg/l N2H4 1441 1441 Hydrazine (Cat. No. 918 44) Wavelength: 436 nm Interferences: No interference will occur due to the presence of foreign matter (e.g. heavy metal ions, neutral salts, ammonia and phosphate ions), which may possibly be present in condensate, feed water or boiler water. The method can also be applied for the analysis of sea water. Procedure: Requisite accessories: piston pipettes with disposable tips, volumetric flasks 25 ml (Cat. No. 916 61) Pour into two separate volumetric flasks: Sample 20 ml test sample, add 2 ml R1, mix, add 2 ml R2, mix Blank value 20 ml dist. water, add 2 ml R1, mix, add 2 ml R2, mix Fill up sample and blank value to 25 ml mark with distilled water, mix again and pour into cuvettes. Clean outside of cuvettes. Reaction time: 10’00 min at 20 – 25 °C Measurement: Call up method 144 Perform measurement Storage: Observe expiry date. If test is not used for some time, we recommend that R2 be stored in a refrigerator and removed in time for the next analysis. If R2 is dark coloured, use a new reagent set. Reference: Thomas / Chamberlin, Colorimetric Chemical Analytical Methods German standard methods for the examination of water, waste water and sludge (DIN 38 413-P1) NANOCOLOR ® – 03/06 Test 1-48 Silica (silicic acid) Method: Standard test Photometric determination of molybdenum blue after reduction of silicomolybdic acid Ranges: 50 mm cuvette Method NANOCOLOR reagent set: 0.01 – 1.40 mg/l Si 0.02 – 3.00 mg/l SiO2 10 mm cuvette 0.05 – 5.00 mg/l Si 0.1 – 10.0 mg/l SiO2 for higher sensitivity see Test 1-483 1481 1482 1481 1482 Silica (Cat. No. 918 48) Wavelength: 690 nm Interferences: Silica contents lower than 0.5 mg/l must be determined against a blank value of silica-free, distilled water with R1, R2 and R3. The following quantities of ions will not interfere: ≤ 10 mg/l Fe, Al ≤ 20 mg/l PO43– ≤ 100 mg/l Ca Please make certain, that the distilled water used for filling up or dilution is free of silica. The method can also be applied for the analysis of sea water. Procedure: Requisite accessories: piston pipettes with disposable tips, volumetric flasks 25 ml (Cat. No. 916 61), silica-free water (Cat. No. 918 912). Pour into two separate volumetric flasks: Sample 20 1 1 1 ml test sample, add ml R1, mix, wait 3 minutes, add ml R2, mix, wait 1 minute, add ml R3 Blank value 20 ml test sample – – – Fill up sample and blank value to 25 ml mark with distilled, silica-free water, mix again and pour into cuvettes. Clean outside of cuvettes. Reaction time: 15’00 min Measurement: Call up method 148 Perform measurement Reference: German standard methods for the examination of water, waste water and sludge (DIN 38 405-D21) NANOCOLOR ® – 03/06 Test 1-483 Silica (high sensitivity) Standard test Method: Photometric determination of molybdenum blue after reduction of silicomolybdic acid (high sensitivity method) Ranges: 50 mm cuvette NANOCOLOR reagent set: Silica (Cat. No. 918 48) Wavelength: 800 nm Interferences: The following quantities of ions will not interfere: ≤ 10 mg/l Fe, Al ≤ 20 mg/l PO43– ≤ 100 mg/l Ca Please make certain, that the distilled water which is used for filling up or dilution, is free of silica. The method can also be applied for the analysis of sea water. Procedure: Requisite accessories: piston pipettes with disposable tips, volumetric flasks 25 ml (Cat.No. 916 61), silica-free water (Cat. No. 918 912). Pour into two separate volumetric flasks: Method Sample 20 ml test sample, add 1 ml R1, mix wait 3 minutes, add 1 ml R2, mix wait 1 minute 1 ml R3 0.002 – 0.100 mg/l Si 0.005 – 0.200 mg/l SiO2 1483 1484 Blank value 20 ml silica-free water, add 1 ml R1, mix wait 3 minutes, add 1 ml R2, mix wait 1 minute 1 ml R3 Fill up sample and blank value to 25 ml mark with distilled, silica-free water, mix again and pour into cuvettes. Clean outside of cuvettes. Reaction time: 15’00 min Measurement: Call up method 148 Perform measurement Reference: German standard methods for the examination of water, waste water and sludge (DIN 38 405-D21) NANOCOLOR ® – 03/06 Test 1-51 Cobalt Standard test Method: Photometric determination with 4-(5-chloro-2-pyridyl-azo)-m-phenylene diamine (5-Cl-PADAB) Ranges: 50 mm cuvette 10 mm cuvette Method NANOCOLOR reagent set: 0.002 – 0.300 mg/l Co2+ 0.02 – 0.70 mg/l Co2+ 1511 1511 Cobalt (Cat. No. 918 51) Wavelength: 540 nm Interferences: Strongly acidic and buffered test samples are to be adjusted to pH 6 before the determination. Total cobalt can be determined with NanOx Metal (Cat. No. 918 978) or with Crack Set (Cat. No. 918 08). The following quantities of ions will not interfere: ≤ 25 mg/l Fe, Ni, Mn ≤ 5 mg/l Cr(VI), Zn, Al ≤ 1 mg/l Cu, Cr(III) The method can also be applied for the analysis of sea water. Procedure: Requisite accessories: piston pipettes with disposable tips, volumetric flasks 25 ml (Cat. No. 916 61) Pour into two separate volumetric flasks: Sample 20 1 1 1 ml test sample, add ml R1, mix, add ml R2, mix, add ml R3, mix Blank value 20 1 1 1 ml dist. water, add ml R1, mix, add ml R2, mix, add ml R3, mix Fill up sample and blank value to 25 ml mark with distilled water, mix again and pour into cuvettes. Clean outside of cuvettes. Reaction time: 5’00 min Measurement: Call up method 151 Perform measurement Reference: Fries/Getrost, Organic reagents for trace analysis NANOCOLOR ® – 03/06 Test 1-53 Method: Ranges: NANOCOLOR reagent set: Copper Standard test Photometric determination with cuprizone 50 mm cuvette 10 mm cuvette 0.01 – 2.00 mg/l Cu2+ 0.1 – 10.0 mg/l Cu2+ Method 1531 1531 Copper (Cat. No. 918 53) Wavelength: 585 nm Interferences: Cr(III) ions interfere (oxidation to chromate using NanOx Metal). Only Cu2+ ions are covered by this test. For the determination of total copper refer to NanOx Metal (Cat. No. 918 978) or Crack Set (Cat. No. 918 08) for sample pretreatment. The following quantities of ions will not interfere: ≤ 100 mg/l Ca ≤ 50 mg/l Co, PO43– ≤ 10 mg/l Fe, Mn, Ni, Zn, Cr(VI) The method can also be applied for the analysis of sea water. Note: For eliminating interfering calcium (up to 20 mg/l Ca2+) use Reagents for lime precipitation (Cat. No. 918 939) For the determination of copper in electroplating baths contact MACHEREYNAGEL for special working instructions. Procedure: Requisite accessories: piston pipettes with disposable tips, volumetric flasks 25 ml (Cat. No. 916 61) Pour into two separate volumetric flasks Sample 20 ml test sample, add 2 ml R1, mix. The pH value has to be between 8.5 and 9.5, otherwise add more R1. Add 2 ml R2, mix Blank value 20 ml test sample – – Fill up sample and blank value to 25 ml mark with distilled water, mix again and pour into cuvettes. Clean outside of cuvettes. The reaction must take place at 20 – 25 °C. Reaction time: 15’00 min Measurement: Call up method 153 Perform measurement Analytical quality control: NANOCONTROL multistandard Metals 2 (Cat. No. 925 016) Reference: Fries/Getrost, Organic reagents for trace analyses NANOCOLOR ® – 03/06 Test 1-60 Manganese Standard test Method: Photometric determination of total manganese with formaldoxime Ranges: 50 mm cuvette 10 mm cuvette Method 0.01 – 2.00 mg/l Mn 0.1 – 10.0 mg/l Mn 16 0/ 1 16 0/ 1 NANOCOLOR reagent set: Manganese (Cat. No. 918 60) Wavelength: 470 nm Interferences: Nickel interferes with the determination of manganese (can be masked with 10 mg potassium cyanide per test). The following quantities of ions will not interfere: ≤ 300 mg/l Ca, Mg ≤ 100 mg/l Zn, PO43– ≤ 10 mg/l Fe ≤ 5 mg/l PO43– when Ca ions are present too. ≤ 1 mg/l Cr, Co, Cu The method can also be applied for the analysis of sea water. Procedure: Requisite accessories: piston pipettes with disposable tips, volumetric flasks 25 ml (Cat. No. 916 61) Pour into two separate volumetric flasks: Sample 20 1 1 1 1 ml test sample, add ml R1, mix, add ml R2, mix, wait 1 minute, add ml R3, mix, add spoon R4 Blank value 20 ml test sample – – – – Fill up sample and blank value to 25 ml mark with distilled water, mix again and pour into cuvettes. Clean outside of cuvettes. Reaction time: 5’00 min Measurement: Analytical quality control: Reference: NANOCOLOR ® – 03/06 Call up method 16 0/ Perform measurement NANOCONTROL multistandard Drinking water (Cat. No. 925 018) Thomas / Chamberlin, Colorimetric Chemical Analytical Methods German standard methods for the examination of water, waste water and sludge (DIN 38 406-E2) Test 1-62 Method: Ranges: NANOCOLOR reagent set: Nickel Standard test Photometric determination with diacetyl dioxime after oxidation to nickel(III) 50 mm cuvette 10 mm cuvette 0.01 – 2.00 mg/l Ni2+ 0.1 – 10.0 mg/l Ni2+ Method 1621 1621 Nickel (Cat. No. 918 62) Wavelength: 436 nm Interferences: Nickel cyanide and nickel cyano complexes are not determined by this test. For the determination of total nickel refer to NanOx Metal (Cat. No. 918 978) or Crack Set (Cat. No. 918 08) for sample pretreatment. ^ 0.02 mg/l Ni Copper interferes: 1 mg/l Cu = The following quantities of ions will not interfere: ≤ 1 mg/l Co, Mn ≤ 5 mg/l Cr ≤ 20 mg/l Fe ≤ 100 mg/l Ca, Zn The method can also be applied for the analysis of sea water. Note: For eliminating interfering calcium (up to 20 mg/l Ca2+) use Reagents for lime precipitation (Cat. No. 918 939) For the determination of nickel in electroplating baths contact MACHEREYNAGEL for special working instructions. Procedure: Requisite accessories: piston pipettes with disposable tips, volumetric flasks 25 ml (Cat. No. 916 61) Pour into two separate volumetric flasks: Sample 20 1 1 1 1 ml test sample, add ml R1 and ml R2, mix, add ml R3, mix, add ml R4, mix Blank value 20 ml test sample – – – – Note: the yellow colouration formed by the addition of R2 must disappear with the addition of R3. Fill up sample and blank value to 25 ml mark with distilled water, mix again and pour into cuvettes. Clean outside of cuvettes. Reaction time: 5’00 min Measurement: Analytical quality control: Reference: NANOCOLOR ® – 03/06 Call up method 162 Perform measurement NANOCONTROL multistandard Metals 2 (Cat. No. 925 016) German standard methods for the examination of water, waste water and sludge (E 11 to 1991) Test 1-63 Nitrate Z Standard test Method: Photometric determination with sulphanilic acid and 1-naphthylamine after reduction to nitrite Ranges: 50 mm cuvette Method 10 mm cuvette NANOCOLOR reagent set: 0.02 – 0.45 mg/l NO3-N 0.1 – 2.0 mg/l NO3– 0.1 – 1.0 mg/l NO3-N 0.5 – 5.0 mg/l NO3– 1631 1632 1631 1632 Nitrate Z (Cat. No. 918 63) Wavelength: 520 nm Interferences: Nitrite interferes (same reaction). This can be circumvented by addition of amidosulphonic acid (Cat. No. 918 973) before nitrate determination. Organic colloids, humic acids, heavy metals, oxidising and reducing substances interfere. The following quantities of ions will not interfere: ≤ 1 mg/l CrO42– ≤ 5 mg/l Fe, Zn, Cl– ≤ 50 mg/l Al, Ca ≤ 100 mg/l SO42–, PO43– If the above concentrations are exceeded (e.g. higher chloride levels), it may still be possible to determine the nitrate content after dilution of the test sample. The method cannot be applied for the analysis of sea water. Procedure: Requisite accessories: piston pipettes with disposable tips, volumetric flasks 25 ml (Cat. No. 916 61) Pour into two separate volumetric flasks: Sample 20 ml test sample, add 1 ml R1, mix, add 1 microspoon of R2, shake for 15 – 30 seconds Blank value 20 ml dist. water, add 1 ml R1, mix, add 1 microspoon of R2, shake for 15 – 30 seconds Fill up sample and blank value to 25 ml mark with distilled water, mix again and pour into cuvettes (R2 will not completely dissolve and forms a deposit). Clean outside of cuvettes. Reaction time: 10’00 min Measurement: Call up method 163 Perform measurement Reference: Zimmermann, Photometric Metal and Water Analyses (B-a 2/1) NANOCOLOR ® – 03/06 Test 1-65 Nitrate Standard test Method: Photometric determination with 2,6-dimethylphenol in sulphuric acid / phosphoric acid mixture Ranges: 10 mm cuvette NANOCOLOR reagent set: Nitrate (Cat. No. 918 65) Method 0.5 – 30.0 mg/l NO3-N 2.0 – 140.0 mg/l NO3– 1651 1652 Wavelength: 365 nm Interferences: Nitrite interferes > 1 mg/l (check with QUANTOFIX® Nitrite – Cat. No. 913 11). This can be circumvented by addition of 1 spoon of amidosulphonic acid (Cat. No. 918 973) to 10 ml test sample. Wait 10 min to determine nitrate. The following ions will not interfere: ≤ 1000 mg/l chloride and carbonate The method cannot be applied for the analysis of sea water. Procedure: Requisite accessories: test tubes, piston pipettes with tips Sample Blank value Place into a test tube1) 4.0 ml Nitrate R1 0.5 ml test sample and 0.5 ml Nitrate R2. Mix by shaking gently. (Test tube becomes hot!) Place into a test tube1) 4.0 ml Nitrate R1 0.5 ml distilled water and 0.5 ml Nitrate R2. Mix by shaking gently. (Test tube becomes hot!) (Blank value stable for 30 min) We recommend VISOCOLOR ® ECO glasses (Cat. No. 931 151) that can be sealed with screw caps thus enabling the sample to be mixed safely. Pour the contents of the test tubes into 10 mm cuvettes (Attention! Hot acidic mixture!). Clean outside of cuvettes. Reaction time: 10’00 min 1) Measurement: Analytical quality control: Reference: NANOCOLOR ® – 03/06 Call up method 165 Perform measurement NANOCONTROL Multistandard Sewage outflow (Cat. No. 925 011) or Sewage influx (Cat. No. 925 012) German standard methods for the examination of water, waste water and sludge (DIN 38 405-D9-2) Test 1-67 Nitrite Method: Standard test Photometric determination with sulphanilic acid and 1-naphthylamine Ranges: 50 mm cuvette Method 10 mm cuvette NANOCOLOR reagent set: 0.002 – 0.100 mg/l NO2-N 0.005 – 0.250 mg/l NO2– 0.01 – 0.30 mg/l NO2-N 0.10 – 1.00 mg/l NO2– 1671 1672 1671 1672 Nitrite (Cat. No. 918 67) Wavelength: 520 nm Interferences: Free chlorine, organic colloids and humic acids interfere. For removal of such interferences take a 100 ml sample, adjust pH value to 8.5 (to avoid adsorption of nitrite ions by activated charcoal), add 1 – 2 g nitrite-free activated charcoal, shake and filter. The method can also be applied for the analysis of sea water. For removal of emulsions, turbidities and colour prior to the test, e.g. for nitrite in cooling lubricants, seepage water from waste deposits etc., use Reagents for sample preparation by clarification precipitation (Cat. No. 918 937). Note: Procedure: Requisite accessories: piston pipettes with disposable tips, volumetric flasks 25 ml (Cat. No. 916 61) Pour into two separate volumetric flasks: Sample 20 ml test sample, add 2 ml R1, mix, add 2 ml R2, mix Blank value 20 ml dist. water, add 2 ml R1, mix, add 2 ml R2, mix Fill up sample and blank value to 25 ml mark with distilled water, mix again, and pour into cuvettes. Clean outside of cuvettes. Reaction time: 10’00 min Measurement: Call up method 167 Perform measurement Analytical quality control: NANOCONTROL Nitrite (Cat. No. 925 68) Reference: Thomas / Chamberlin, Colorimetric Chemical Analytical Methods NANOCOLOR ® – 03/06 Test 1-75 Method: Phenol Standard test Photometric determination with diazotised 4-nitroaniline Method Ranges: NANOCOLOR reagent set: 50 mm cuvette 10 mm cuvette 0.01 – 1.00 mg/l Phenol 0.1 – 7.0 mg/l Phenol 1751 1751 Phenol (Cat. No. 918 75) Wavelength: 470 nm Interferences: Apart from phenol, most other phenol derivatives are also determined (sometimes with different colourations). In case of water, which is heavily contaminated with organic compounds, the phenols should first be separated by steam distillation. The method can also be applied for the analysis of sea water after dilution (1:10). Procedure: Requisite accessories: piston pipettes with disposable tips, volumetric flasks 25 ml (Cat. No. 916 61) Pour into two separate volumetric flasks: Sample 1 ml R1 add a few crystals of R2, until solution is colourless, add 20 ml test sample, mix 1 ml R3, mix Blank value 1 ml R1 add a few crystals of R2, until solution is colourless, add 20 ml dist. water, mix 1 ml R3, mix Fill up sample and blank value to 25 ml mark with distilled water, mix again and pour into cuvettes. Clean outside of cuvettes. Reaction time: 5’00 min Measurement: Call up method 175 Perform measurement Reference: German standard methods for the determination of water, waste water and sludge (H 16 until 1984) NANOCOLOR ® – 03/06 Test 1-77 ortho-Phosphate Method: Standard test Photometric determination as phosphormolybdenum blue Ranges: 50 mm cuvette Method 10 mm cuvette 0.04 – 1.70 mg/l PO4-P 0.1 – 5.0 mg/l PO43– 0.2 – 6.5 mg/l PO4-P 0.5 – 20.0 mg/l PO43– 1771 1772 1771 1772 NANOCOLOR reagent set: ortho-Phosphate (Cat. No. 918 77) Wavelength: 690 nm Interferences: For the determination of total phosphorus use tests 0-76, 0-79, 0-80 or 0-81 or NanOx Metal (Cat. No. 918 978). The following quantities of ions will not interfere: ≤ 10 mg/l SiO2, Fe, Pb, Zn ≤ 200 mg/l Ca, citrate, tartrate Use only repeatedly and thoroughly rinsed glassware. The method can also be applied for the analysis of sea water. Note: For the determination of phosphate in sludge contact MACHEREY-NAGEL for special working instructions. Procedure: Requisite accessories: piston pipettes with disposable tips, volumetric flasks 25 ml (Cat. No. 916 61) Pour into two separate volumetric flasks: Sample 20 ml test sample and 1 ml R1, mix, add 1 ml R2, mix Blank value 20 ml dist. water and 1 ml R1, mix, add 1 ml R2, mix Fill up sample and blank value to 25 ml mark with distilled water, mix again and pour into cuvettes. Clean outside of cuvettes. Reaction time: 10’00 min Measurement: Call up method 177 Perform measurement Analytical quality control: NANOCONTROL ortho-Phosphate (Cat. No. 925 76) Reference: Thomas / Chamberlin, Colorimetric Chemical Analytical Methods NANOCOLOR ® – 03/06 Test 1-78 ortho-Phosphate Standard test Method: Photometric determination of the yellow phosphate-molybdate-vanadate complex in acidic solution. Ranges: 50 mm cuvette Method 10 mm cuvette NANOCOLOR reagent set: 0.2 – 6.6 mg/l PO4-P 0.5 – 20.0 mg/l PO43– 0.4 – 15.0 mg/l P2O5 1 – 17 mg/l PO4-P 2 – 50 mg/l PO43– 1.5 – 37.0 mg/l P2O5 1781 1782 1783 1781 1782 1783 ortho-Phosphate (Cat. No. 918 78) Wavelength: 436 nm Interferences: For the determination of total phosphorus use tests 0-76, 0-79, 0-80 or 0-81 or NanOx Metal (Cat. No. 918 978). < 10 mg/l iron do not interfere. Silicate ions in larger quantities also do not interfere when the test solution is acidified sufficiently. Use only repeatedly and thoroughly rinsed glassware. The method can also be applied for the analysis of sea water. Procedure: Requisite accessories: piston pipettes with disposable tips, volumetric flasks 25 ml (Cat. No. 916 61) Pour into two separate volumetric flasks: Sample 20 ml test sample and 1 ml R1, mix, add 1 ml R2, mix Blank value 20 ml dist. water and 1 ml R1, mix, add 1 ml R2, mix Fill up sample and blank value to 25 ml mark with distilled water, mix again and pour into cuvettes. Clean outside of cuvettes. Reaction time: 10’00 min Measurement: Call up method 178 Perform measurement Reference: Thomas / Chamberlin, Colorimetric Chemical Analytical Methods NANOCOLOR ® – 03/06 Test 1-88 Sulphide Standard test Method: Photometric determination as methylene blue Ranges: 50 mm cuvette 10 mm cuvette Method 0.01 – 0.60 mg/l S2– 0.1 – 3.0 mg/l S2– 1881 1881 NANOCOLOR reagent set: Sulphide (Cat. No. 918 88) Wavelength: 620 nm Interferences: Sulphide concentration is measured in an acidic medium and therefore if the reagents are not mixed gently, some sulphide may escape as hydrogen sulphide, leading to lower test results. The following quantities of ions will not interfere: ≤ 10 mg/l SCN–, SO32– ≤ 100 mg/l NO2– The method can also be applied for the analysis of sea water. Procedure: Requisite accessories: piston pipettes with disposable tips, volumetric flasks 25 ml (Cat. No. 916 61) Pour into two separate volumetric flasks: Sample 20 ml test sample, add 1 microspoon R1, shake gently, wait 1 minute, hold volumetric flask at an angle and pour down the inner side 1 ml R2, shake briefly, add 1 ml R3 Blank value 20 ml test sample – – – Fill up sample and blank value to 25 ml mark with distilled water, mix again and pour into cuvettes. Clean outside of cuvettes. Reaction time: 5’00 min Measurement: Call up method 188 Perform measurement Reference: German standard methods for the examination of water, waste water and sludge (DIN 38 405-D26/D27) NANOCOLOR ® – 03/06 Test 1-92 Turbidity (DIN or Formazine) Standard test Method: Photometric determination of the turbidity in comparison to formazine standard suspensions Ranges: 50 mm cuvette Method 1 – 100 FAU (Formazine attenuation units) 1921 Spectral absorbance coefficient in accordance with the German standard methods 0.5 – 40.0 1/m (at 620 nm, ∆ λ = 10 nm) 1922 For measurement at 860 nm (DIN EN 27027) contact MACHEREY-NAGEL Wavelength: 620 nm Interferences: Green colourations (600 – 640 nm) simulate turbidity. The method can also be applied for the analysis of sea water. Procedure: Pour into two separate dry cuvettes Sample Blank value test sample distilled water Measurement: Call up method 192 Perform measurement Reference: German standard methods for the examination of water, waste water and sludge (DIN EN ISO 7027-C2) NANOCOLOR ® – 03/06 Test 1-95 Method: Ranges: NANOCOLOR reagent set: Zinc Standard test Photometric determination with zincon 50 mm cuvette 10 mm cuvette 0.02 – 1.50 mg/l Zn2+ 0.1 – 3.0 mg/l Zn2+ Method 1951 1951 Zinc (Cat. No. 918 95) Wavelength: 620 nm Interferences: Acidic, basic and buffered test samples should be adjusted to pH 9 after addition of R2. If after addition of R2 the sample becomes turbid, the contents of the volumetric flask have to be centrifuged or filtered prior to the measurement (membrane filters 0.45 µm, Cat. No. 916 50). Only Zn(II) ions are determined. For the determination of total zinc refer to NanOx Metal (Cat. No. 918 978) or Crack Set (Cat. No. 918 08) for sample pretreatment. The chromium(III) concentration must not exceed the zinc concentration. Higher chromium(III) amounts result in falsely low results (oxidation to chromate with NanOx Metal). The following quantities of ions will not interfere: < 1000 mg/l Ca2+, Cl–, SO42–; < 500 mg/l Cr(VI); < 200 mg/l Mg2+; < 50 mg/l Ni2+; < 10 mg/l PO43–; < 5 mg/l Al3+, Cu2+; < 1 mg/l Cd2+, Fe3+; < 0.1 mg/l Mn2+ For large amounts of calcium and for higher manganese concentrations contact MACHEREY-NAGEL for special working instructions. The method can also be applied for the analysis of sea water after dilution (1+9). Procedure: Requisite accessories: piston pipette with disposable tips, volumetric flasks 25 ml (Cat.No. 916 61) Pour into two separate volumetric flasks: Sample 20 ml test sample 1 ml R1, mix, 1 ml R2, mix, check pH (8.5 – 9.5) wait 2 min 1 ml R3, do not mix Blank value 20 ml dist. water 1 ml R1, mix, 1 ml R2, mix, wait 2 min 1 ml R3, do not mix Fill up sample and blank value to 25 ml mark with distilled water, mix and pour into cuvettes. Clean outside of cuvettes. Reaction time: 1’00 min Measurement: Analytical quality control: Reference: NANOCOLOR ® – 03/06 Call up method 195 Perform measurement NANOCONTROL multistandard Metals 1 (Cat. No. 925 015) Fries/Getrost, Organic reagents for trace analyses Schwarzenbach, Complexometric titration