QC 8000 REAGENT RECIPES
GEL Revision Date:
3 August 2004
Index
Alkalinity (Methyl Orange)……………………………………………………………..3
Ammonia………………………………………………………………………………….4
Bromide…………………………………………………………………………………..8
Chloride………………………………………………………………………….……...10
Nitrate/Nitrite……………………………………………………………………..…….11
Orthophosphate…………….…………………………………………………………..13
Sulfate…………………………………………………………………………………...16
Sulfate (Low flow)……………………………………………………………………....19
Total Nitrogen…………………………………………………………………………..22
Total Phosphate………………………………………………………………………....25
General Notes:
1. GEL revisions are indicated by italics.
2. For different quantities, the respective amounts are given in parentheses or
brackets.
3. Use Nanopure deionized water (>M ohm-cm) for all solutions specifying water as
solvent.
4. Degassing with helium:
To prevent bubble formation, degas water before preparing solutions with helium.
Use He at 140 kPa (20 lb/in2) through a helium degassing tube (Lachat Part No.
50100). Bubble He through the water for several minutes.
5. Chemical and reagent locations:
DC
Dry Chemical Cabinet (GWC 675)
SC
Standards Cabinet (GWC 675)
WIR Walk-in Refrigerator (GWC 675)
AC
Acid Cabinet (GWC 675)
BC
Base Cabinet (GWC 675)
OC
Organic Solvent Cabinet (GWC 675)
RC
Reagent Cabinet (GWC 637)
2
QuickChem® METHOD 10-303-31-1-A
DETERMINATION OF ALKALINITY (METHYL ORANGE) IN SURFACE AND
WASTEWATERS BY FLOW INJECTION ANALYSIS
COLORIMETRY
21 December 1998
List of Raw Materials
Hydrochloric Acid (HCl) – CAS 7647-01-0, (DC 675)
Methyl Orange (indicator grade, Aldrich #11,451-0) – CAS #, (DC 675)
Potassium Acid Phthalate [Potassium Hydrogen Phthalate, Potassium biphthalate, KHP],
(HOOCC6, H4COOK) – CAS 877-24-7, (DC 675)
Carbon dioxide-free water
Bring 6 L of water to a boil for five minutes to remove carbon dioxide. Cool
before using to avoid error in the volumetric measurements.
Reagent 1. Hydrochloric Acid (HCl), 0.1M
By Volume: In a 1 L volumetric flask containing about 800 mL carbon dioxidefree water, add 8.3 mL concentrated hydrochloric acid. Dilute to the mark
with carbon-dioxide free water. Invert to mix.
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Reagent 2. KHP Buffer pH 3.1, 25.0 mM (RC 637)
By Volume: In a 1 L container, dissolve 5.0 g potassium acid phthalate
[potassium hydrogen phthalate, potassium biphlalate, KHP, (HOOCC6
H4COOK)] in 900 mL carbon dioxide-free water. Add 85.0 mL 0.1 M HCl
(reagent 1), then add acid (no more than 5.0 mL) to bring the pH to 3.1 +/- 0.05.
If greater then 5.0 mL of 0.1 M HCl is necessary, start over in the preparation of
this reagent. If this fails, use Standardized 0.1 M HCl. Pour into a glass storage
bottle. Prepare fresh weekly.
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3
Reagent 3. Methyl Orange Reagent (RC 637)
By Volume: In a 1 L volumetric flask, dissolve 0.1313 g methyl orange
(indicator grade, Aldrich #11,451-0) in about 700 mL carbon dioxide-free
water. Dilute to the mark and invert to mix. Store in glass. Use indicator grade
methyl orange.
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4
QuickChem Method 10-107-06-1-J
DETERMINATION OF AMMONIA BY FLOW INJECTION ANALYSIS
15 March 2001
List of Raw Materials
Disodium Ethylenediamine Tetraacetic Acid (Na2EDTA) - CAS 6381-92-6, (DC)
Phenol (C6H5OH), crystalline – CAS 108-95-2, (WIR)
Sodium Hydroxide (NaOH) – CAS 1310-73-2, (BC)
Sodium Hypochlorite (NaOCl), Commercial grade; e.g. Clorox institutional &
germicidal, (WIR)
Sodium Nitroprusside [Sodium Nitroferricyanide] (Na2Fe(CN)5NO·2H2O) –
CAS 13755-38-9, (DC)
Sulfuric Acid (H2SO4) – CAS 7664-93-9, (DC)
Reagent 1. Sodium Phenolate (RC 637)
*Add Phenol last. (Use also for TRAACS) Add NaOH to a portion of the H2O and allow
to cool. Use the remainder of H2O to rinse in phenol.
CAUTION: Wear gloves. Phenol causes severe burns and is rapidly absorbed into the
body through the skin.
By Volume: In a 1 (0.5) [0.25] L volumetric flask, dissolve 83 (41.5) [20.75] g
crystalline phenol (C6H5OH) is approximately 600 (300) [150] mL DI water.
While stirring, slowly add 32 (16) [8] g sodium hydroxide (NaOH). Cool, dilute
to the mark and invert to mix. Do not degas this reagent. Prepare fresh every 3
to 5 days. Discard when reagent turns brown. *Use solid NaOH for N
determination in base cabinet.
By Weight: QC 8000-Good Baseline. To a tared 1 (0.5) L container, add 888
(444) g DI water. Add 83 (41.5) g crystalline phenol (C6H5OH). While stirring,
slowly add 32 (16) g sodium hydroxide (NaOH). Cool and invert to mix
thoroughly. Do not degas this reagent. Prepare fresh every 3 to 5 days. Discard
when reagent turns brown. *Use solid NaOH for N determination in base
cabinet.
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5
Reagent 2. Sodium Hypochlorite
*Use 30 mL Clorox/70mL water
By Volume: In a 500 mL volumetric flask, dilute 214 mL 5.25% sodium
hypochlorite (NaOCl) to the mark with DI water. Invert to mix. Prepare fresh
daily.
*@ 3% sodium hypochlorite use 175 mL bleach and 25 mL water.
*Use small bottle of bleach on counter in walk in – old JT Baker bottle. Refill it
from large bleach bottle under sink in walk in.
* 70 ml of water to 30 mL of bleach – WJR 10/7/02
By Weight: To a tared 500 mL container add 214 g 5.25% sodium
hypochlorite (NaOCl) and 250 g DI water. Stir or shake to mix. Prepare fresh
daily.
Note: If Clorox bleach is not available solid sodium hypochlorite can be
substituted. Dilute 26.25 g sodium hypochlorite to 500 mL with DI water.
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Reagent 3. Sodium Nitroprusside (RC 637)
By Volume: In a 1 (0.5) L volumetric flask, dissolve 0.5 (0.25) g sodium
nitroprusside (sodium nitroferricyanide [Na2Fe(CN)5NO·2H2O]). Dilute to the
mark with DI water and invert to mix. Store in a light resistant container.
Prepare fresh every 1 to 2 weeks.
By Weight: To a tared 1 L container add 0.5 g sodium nitroprusside (sodium
nitroferricyanide [Na2Fe(CN)5NO·2H2O]) and 1000 g DI water. Invert to mix.
Store in a light resistant container. Prepare fresh every 1 to 2 weeks.
* Use TrAAcs concentration 0.5g in 1L
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Reagent 4. 1 M Sodium Hydroxide Solution
By Volume: In a 1 L volumetric flask, dissolve 40.0 g sodium hydroxide
(NaOH) in approximately 900 mL DI water. Dilute to the mark and mix with a
magnetic stirrer until dissolved. *Use solid NaOH for N determination in base
cabinet.
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6
Reagent 5. Buffer for Non Acid Preserved Samples (RC 637)
By Volume: In a 1 (0.5) L volumetric flask, dissolve 50.0 (25) g disodium
ethylenediamine tetraacetic acid (Na2EDTA) and 225 (117.5) mL 1 M sodium
hydroxide (Reagent 4) (or 15 mL 15 M NaOH or use 9 g solid NaOH*) in
approximately 700 (350) mL DI water. Dilute to the mark and mix with a
magnetic stirrer until dissolved. Prepare fresh monthly.
* Use the NaOH in base cabinet for nitrogen determination (9 (4.5) g is for prep
of 1 (0.5) L of buffer). --CK 03/01/01
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If the samples are preserved at a pH less than two with sulfuric acid, the following
reagent and standard recipe changes apply:
Reagent 6. Buffer for Acid Preserved Samples (RC 637)
By Volume: In a 1 L volumetric flask, dissolve 50.0 g disodium
ethylenediamine tetraacetic acid (Na2EDTA) and 254 mL 1 M sodium
hydroxide (NaOH) solution (Reagent 4) [10.16 g solid NaOH for 1 L or 5.08 g
for 500 mL] in approximately 700 mL DI water. Dilute to the mark and mix
with a magnetic stirrer until dissolved. Prepare fresh monthly.
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Reagent 7. Sulfuric Acid Diluent for Carrier and Standards (Acid preserved samples
only)
By Volume: In a 1 L volumetric flask, add approximately 800 mL DI water
followed by 2 mL concentrated sulfuric acid. Dilute to the mark. Keep flask
sealed when not in use with parafilm to avoid ambient ammonia contamination.
NOTES:
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7
QuickChem Method 10-135-21-2-A
DETERMINATION OF BROMIDE IN WATERS BY FLOW INJECTION
ANALYSIS
List of Raw Materials
Acetic Acid (glacial) – CAS 64-19-7, (AC 675)
Chloramine-T – CAS 7080-50-4, (DC 675)
Phenol Red – CAS 143-74-8, (DC 675)
Sodium Acetate – CAS 127-09-3, (DC 675)
PREPARATIONS OF REAGENTS
Use deionized water (10 megohm) for all solutions
Degassing with helium:
To prevent bubble formation, degas all solutions except the standards with
helium. Use He at 140 kPa (20 lb/in2) through a helium degassing tube (Lachat
Part No. 50100). Bubble He through the solution for one minute.
Reagent 1. Chloramine-T Color Reagent
By Volume: In a 1 (0.5) [0.25] L volumetric flask, add 0.80 (0.40) [0.20] g
chloramine-T. Add water to the mark. Invert flask six times. Inversion will
dissolve the chloramine-T. Do not use a magnetic stirrer. Prepare fresh daily.
By Weight: To a tared 1 (0.5) [0.25] L container, add 0.80 (0.40) [0.20] g
chloramine-T and 999 (499.5) [249.75] g water. Invert the container six times.
Inversion will dissolve the chloramine-T. Do not use a magnetic stirrer. Prepare
fresh daily. NOTE: Dry chloramine-T reagent is good for 6 months.
Reagent 2. Phenol Red Color and Buffer Reagent
By Volume: In a 1 (0.5) [0.25] L volumetric flask, add approximately 600 mL
water. Add 29.0 (14.5) [7.25] mL glacial acetic acid. Swirl contents of flask.
Add 41.0 (20.5) [10.25] g sodium acetate. Swirl contents until dissolved. Add
0.040g (0.020) [0.010] phenol red (water soluble). Swirl contents until dissolved.
Add water to the mark. Mix with a magnetic stirrer.
By Weight: To a tared 1 L (0.5) [0.25] container, add 929 (464.5) [232.25] g
water and 30.0 (15.0) [7.5] g glacial acetic acid. Swirl contents of container. Add
41.0 (20.5) [10.25] g sodium acetate. Swirl contents of container until dissolved.
Add 0.040 (0.020) [0.010] g phenol red (water soluble). Mix with a magnetic
stirrer.
8
Reagent 3. Amberlite XAD-2 Column Preparation
1. Prepare approximately 1.0 g Amberlite XAD-2 resin, 20-60 mesh, by mixing
with 10 mL water to make a slurry.
2. Remove one end fitting from the glass column (Lachat Part No. 50232).
Clamp the column vertically to a ring stand with the open end of the column
facing upward. Attach a small plastic funnel to the top of the column with
Tygon tubing. Attach a six inch piece of Tygon tubing to the nozzle of a 10.0
mL plastic syringe and attach the other end of Tygon tubing to the bottom of
the column. Fill the column with water. Pour the Amberlite resin slurry into
the plastic funnel. Slowly draw back on the plastic syringe in order to draw
the water and Amberlite resin into the glass column. Avoid trapping air
bubbles in the column or its fittings.
3. When the resin has settled, replace the end fitting. To ensure a good seal,
remove any resin particles from the threads of the glass, the column end, and
the end fitting. To store the column, join the ends of the Teflon tubing with a
union.
NOTES:
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9
QuikChem® METHOD 10-117-07-01-H
QuikChem® METHOD 10-117-07-01-I
DETERMINATION OF CHLORIDE BY FLOW INJECTION ANALYSIS
COLORIMETRY
All Ranges
13 December 1994
List of Raw Materials
Ferric Nitrate (Fe(NO3)3·9H2O) – CAS 7782-61-8, (DC 675)
Mercuric Thiocyanate (Hg(SCN)2) – CAS 592-85-8, (DC 675)
Methanol (CH3OH) – CAS 67-56-1, (OC 675)
Reagent 1. Combined Color Reagent
A. Stock Mercuric Thiocyanate Solution (Use also for TRAACS) (RC 637)
In a 1 (0.25) L volumetric flask, dissolve 4.17 (1.042) g mercuric thiocyanate
(Hg(SCN) 2) to about 500 (125) mL methanol. Dilute to the mark with methanol
and mix.
CAUTION: Mercuric thiocyanate is toxic. Wear gloves!
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B. Stock Ferric Nitrate Reagent, 0.5 M (Use also for TRAACS) (RC 637)
In a 1 L volumetric flask, dissolve 202 g ferric nitrate (Fe(NO3)3·9H2O) in
approximately 800 mL water. Add 25 mL 65% concentrated nitric acid and
dilute to the mark. Invert to mix.
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C. Combined Color Reagent (Use also for TRAACS) (RC 637)
In a 500 mL volumetric flask, add 75 mL stock mercuric thiocyanate solution
with 75 mL stock ferric nitrate reagent and dilute to the mark with water.
Invert to mix. Vacuum filter through a 0.45 micrometer membrane filter.
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10
QuikChem® METHOD 10-107-04-1-C
QuikChem® METHOD 10-107-04-1-O
DETERMINATION OF NITRATE/NITRITE IN SURFACE AND
WASTEWATERS BY FLOW INJECTION ANALYSIS
All Ranges
23 April 1999
List of Raw Materials
Ammonium Chloride (NH4Cl) – CAS 12125-02-9, (DC 675)
Ammonium Hydroxide (NH4OH) – CAS 1336-21-6, (BC 675)
Disodium EthyleneDiamine Tetraacetic Acid (Na2EDTA) – CAS 6381-92-6, (DC 675)
Hydrochloric Acid (HCl) – CAS 7647-01-0, (AC 675)
N-(1-naphthyl)ethylenediamine dihydrochloride (NED) – CAS 1465-25-4, (DC 675)
Phosphoric Acid (H3PO4) – CAS 7664-38-2, (AC 675)
Sodium Hydroxide (NaOH) – CAS 1310-73-2, (BC 675)
Sulfanilamide – CAS 63-74-1, (DC 675)
Reagent 1. 15 N Sodium Hydroxide
By Volume: Add 150 g NaOH very slowly to 250 ml or g of water.
CAUTION: The solution will get very hot! Swirl until dissolved. Cool and
store in a plastic bottle.
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Reagent 2. Ammonium Chloride buffer, pH 8.5 (hood 637)
By Volume: CAUTION: Fumes!!! In a hood, to a 1 (0.5) L volumetric flask,
add 500 (250) mL water, 105 (52.5) mL concentrated hydrochloric acid (HCl),
95 (47.5)mL ammonium hydroxide (NH4OH), and 1.0 (0.5) g disodium EDTA.
Dissolve and dilute to the mark. Invert to mix. Adjust the pH to 8.5 with HCl or
15 N NaOH solution.
By Volume x2:
1000 mL H2O
210 mL HCl
100 mL rinse H2O
190 mL NH4OH
100 mL rinse H2O
1600 mL
400 mL H2O (Add 2 g EDTA to this solution)
2000 mL NH4Cl Buffer
11
By Weight: CAUTION: Fumes!!! In a hood, to a tared 1 L container, add 800
g water, 126 g concentrated hydrochloric acid (HCl), 85 g ammonium
hydroxide (NH4OH) and 1.0 g disodium EDTA. Stir until dissolved. Adjust the
pH to 8.5 with HCl or 15 N NaOH.
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Reagent 3. Sulfanilamide color reagent (RC 637)
By Volume: To a 1 (0.5 L) L volumetric flask, add about 600 (300) mL water.
Then add 100 (50) mL of 85% phosphoric acid (H3PO4), 40.0 (20) g
sulfanilamide and 1.0 (0.5) g N-(1-naphthylenediamine dihydrochloride
(NED). Shake to wet and stir for 30 minutes to dissolve. Dilute to the mark and
invert to mix. Store in a dark bottle. This solution is stable for one month.
By Weight: To a tared, dark 1 L container, add 876 g water, 170 g 85%
phosphoric acid (H3PO4), 40.0 g sulfanilamide and 1.0 g N-(1naphthyl)ethylenediamine dihydrochloride (NED). Shake until wetted and stir
with stir bar for 30 minutes until dissolved. This solution is stable for one month.
NOTES:
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12
QuikChem® METHOD 10-115-01-1-Q
QuikChem® METHOD 10-115-01-1-A
DETERMINATION OF ORTHOPHOSPHATE IN WATERS BY FLOW
INJECTION ANALYSIS COLORIMETRY
All Ranges
28 December 1998
List of Raw Materials
Ammonium Molybdate Tetrahydrate [(NH4)6Mo7O24·4H2O] – CAS 12054-85-2, (DC 675)
Antimony Potassium Tartrate [Potassium Antimonyl Tartrate Hemihydrate]
(K(SbO)C4H4O6·1/2H2O) – CAS #, (DC 675)
Antimony Potassium Tartrate [Potassium Antimonyl Tartrate Trihydrate]
(K(SbO)C4H4O6·3H2O) – CAS #, (DC 675)
Ascorbic Acid (Spectrum catalog no. AS 102), granular – CAS 50-81-7, (DC 675)
Dodecyl Sulfate, Sodium Salt (CH3(CH2)11OSO3Na) – CAS 151-21-3, (DC 675)
Sodium Hydroxide (NaOH) – CAS 1310-73-2, (BC 675)
Sulfuric Acid (H2SO4) – CAS 7664-93-9, (AC 675)
Tetrasodium Ethylenediamine tetraacetic Acid (Na4EDTA) – CAS #, (DC 675)
Reagent 1. Stock Ammonium Molybdate Solution (RC 637)
By Volume: In a 1 L volumetric flask dissolve 40.0 g ammonium molybdate
tetrahydrate [(NH4) 6Mo7O24·4H2O] in approximately 800 mL water. Dilute to
the mark and stir for two hours. Store in plastic and refrigerate. May be stored up
to two months when kept refrigerated.
By Weight: To a tared 1 L container add 40.0 g ammonium molybdate
tetrahydrate [(NH4) 6Mo7O24·4H2O] and 983 g water. Stir for two hours. Store
in plastic and refrigerate. May be stored up to two months when kept refrigerated.
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Reagent 2. Stock Antimony Potassium Tartrate Solution
By Volume: In a 1 L volumetric flask, dissolve 3.0 antimony potassium
tartrate (potassium antimonyl tartrate hemihydrate K(SbO)C4H4O6·1/2H2O) or
dissolve 3.22 g antimony potassium tartrate (potassium antimonyl tartrate
trihydrate K(SbO)C4H4O6·3H2O) in approximately 800 mL of water. Dilute to
the mark and stir for a minimum of four hours. Store in a dark bottle and
refrigerate. May be stored up to two months when kept refrigerated.
13
By Weight: To a 1 L dark, tared container add 3.0 g antimony potassium
tartrate (potassium antimonyl tartrate hemihydrate K(SbO)C4H4O6·1/2H2O) or
dissolve 3.22 g antimony potassium tartrate (potassium antimonyl tartrate
trihydrate K(SbO)C4H4O6·1/2H2O) and 995 g of water. Stir for a minimum of
four hours. Store in a dark bottle and refrigerate. May be stored up to two
months when kept refrigerated.
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Reagent 3. Molybdate Color Reagent
By Volume: To a 250 (500) [1000] mL volumetric flask add about 125
(250)[500] mL water, then add 8.75 (17.5) [35] mL concentrated sulfuric acid
(CAUTION: The solution will get very hot!). Swirl to mix. When it can be
comfortably handled, add 18 (36) [72] mL Stock Antimony Potassium Tartrate
Solution (Reagent 2) and 53.25 (106.5)[213] mL Stock Ammonium Molybdate
Solution (Reagent 1). Dilute to the mark and invert three times. Prepare fresh
weekly.
By Weight: To a tared 1 L container add 680 g water, then 64.4 g concentrated
sulfuric acid (CAUTION: The solution will get very hot!). Swirl to mix. When
it can be comfortably handled, add 72.0 g Stock Antimony Potassium Tartrate
Solution (Reagent 2) and 213 g Stock Ammonium Molybdate Solution
(Reagent 1). Prepare fresh weekly.
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Reagent 4. Ascorbic Acid Reducing Solution, 0.33 M
By Volume: In a 1 (0.5) [0.25] L volumetric flask dissolve 70 (35) [17.5] g
granular ascorbic acid (Spectrum catalog no. AS 102) in about 700 (350)[175]
mL of water. Dilute to the mark and invert to mix. Add 1.0 (0.5) [0.25] g
dodecyl sulfate, sodium salt (CH3(CH2) 11OSO3Na) (Aldrich catalog no. 86,2100). Prepare fresh weekly. Discard if the solution becomes yellow. Do not use
ascorbic acid powder.
By Weight: To a tared 1 L container, add 60.0 g granular ascorbic acid
(Spectrum catalog As102) and 975 g water. Stir or shake until dissolved. Add
1.0 g dodecyl sulfate, sodium salt (CH3(CH2) 11OSO3Na) (Aldrich catalog no.
86,210-0). Prepare fresh weekly. Discard if the solution becomes yellow. Do
not use ascorbic acid powder.
14
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Reagent 5. Sodium Hydroxide – EDTA Manifold Rinse
Dissolve 65 g sodium hydroxide (NaOH) and 6 g tetrasodium ethylenediamine
tetraacetic acid (Na4EDTA) in 1.0 L or 1.0 kg water. Store in plastic.
NOTES:
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15
QuikChem® METHOD 10-116-10-2-B
DETERMINATION OF HIGH RANGE SULFATE BY FLOW INJECTION
ANALYSIS COLORIMETRY
23 October 2000
List of Raw Materials
Ammonium Chloride (NH4Cl) – CAS 12125-02-9, (DC 675)
Ammonium Hydroxide (NH4OH) – CAS 1336-21-6, (BC 675)
Barium Chloride Dehydrate (BaCl2·2H2O) – CAS #, ( )
Ethanol (CH5OH) – CAS #, ( )
Hydrochloric Acid (HCl) – CAS 7647-01-0, (AC 675)
methylthymol blue {3,3’-bis[N,N-di(carboxymethyl)aminomethyl]-thymolsulfonephthalein, pentasodium salt} (Lachat Part no. 50243, see System Note 11.3.4) –
CAS #, (DC 675)
Sodium Hydroxide (NaOH) – CAS 1310-73-2, (BC 675)
Tetrasodium EDTA Dehydrate (Na4EDTA) – CAS #, ( )
Reagent 1. Carrier, 0.30 mg SO42-/L (RC 637)
By Volume: To a 1 L volumetric flask add 0.30 mL of 1000 mg/L Stock Sulfate
Solution (Standard 1, found in Standards Preparations section). Dilute to the
mark and mix by inverting. Degas with helium.
By Weight: To a tared 1 L container add 0.30 g of 1000 mg/L Stock Sulfate
Solution (Standard 1, found in Standards Preparation section) and 999.7 g water.
Shake or stir to mix. Degas with helium.
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Reagent 2. Barium Chloride Solution, 6.24 mM (RC 637)
By Volume: In a 1 L volumetric flask, dissolve 1.526 g barium chloride
dehydrate (BaCl2·2H2O) and 500 mL water. Shake or stir until dissolved.
Degas with helium.
By Weight: In a 1 L volumetric flask, dissolve 1.526 g barium chloride
dehydrate (BaCl2·2H2O) and 995 g water. Shake or stir until dissolved. Degas
with helium.
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16
Reagent 3. Hydrochloric Acid, 1.0 M
By Volume: In a 1 L volumetric flask add approximately 800 mL water and 83
mL concentrated hydrochloric acid (specific gravity 1.20, 37%). CAUTION:
Fumes! Dilute to the mark and mix by inverting. Degas with helium.
By Weight: To a tared 1 L container add 913 g water and 99.6 g concentrated
hydrochloric acid (specific gravity 1.20, 37%). CAUTION: Fumes! Shake or
stir to mix well. Degas with helium.
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Reagent 4. Barium – MTB Color Reagent
Make at least 1 Day Before Run
Note: In preparing this reagent, we have found that the purity of the
methylthymol blue and the denaturants in the alcohol are critical. USE THE
SOURCES SPECIFIED BELOW, or test the material from alternate sources for
suitability before using.
By Volume: Into a dry 500 (1000) mL volumetric flask place 0.236 (0.472) g
methylthymol blue {3,3’-bis[N,N-di(carboxymethyl)aminomethyl]-thymolsulfonephthalein, pentasodium salt} (Lachat Part no. 50243, see System Note
11.3.4). Add 50 (100)mL Barium Chloride Solution (Reagent 2) which may be
used to aid in the transfer of the dye. Swirl to dissolve. Using a 5 mL Mohr pipet
or a 4.0 mL volumetric pipet, add 4.0 (8.0) mL of the 1.0 M Hydrochloric Acid
Solution (Reagent 3) and mix. The solution should turn orange. Add 71 (142)
mL water and dilute to the mark with ethanol (ethyl alcohol, specially denatured
anhydrous alcohol, Aldrich 24,511-9). Mix by inverting. The pH of this solution
should be 2.5. Prepare this solution the day before use and store it refrigerated in
a brown plastic bottle. Allow to warm to room temperature before using, then
degas with helium. This is good for one week.
By Weight: To a tared 500 mL dry brown plastic bottle, place 0.236 g
methylthymol blue {3,3’-bis[N,N-di(carboxymethyl)aminomethyl]-thymolsulfonephthalein, pentasodium salt}(Lachat Part no. 50243, see System Note
11.3.4). Add 50 g Barium Chloride Solution (Reagent 2) which may be used to
aid in the transfer of the dye. Swirl to dissolve. Add 4.0 g of the 1.0 M
Hydrochloric Acid Solution (Reagent 3) and mix. The solution should turn
orange. Add 71 g water and 321 g ethanol (ethyl alcohol, specially denatured
anhydrous alcohol, Aldrich 24,511-9). Stir or shake to mix well. The pH of this
solution should be 2.5. Prepare this solution the day before use and store it
refrigerated in a brown plastic bottle. Allow to warm to room temperature before
using, then degas with helium.
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17
Reagent 5. Stock Sodium Hydroxide, 50% Solution
By Volume: In a 1 L volumetric flask, cautiously dissolve 500.0 g sodium
hydroxide (NaOH) in about 800 mL water. CAUTION: The solution will get
very hot! Cool to ambient. Dilute to the mark and mix by inversion. Store in a
plastic bottle.
By Weight: To a tared glass 1 L container add 880 g water and 500.0 g sodium
hydroxide (NaOH). CAUTION: The solution will get very hot! Shake or stir
until dissolved. Cool to ambient. Store in a plastic bottle.
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Reagent 6. Working Sodium Hydroxide , 0.18 M (RC 637)
By Volume: Using a 25 mL graduated cylinder add 14.4 (7.2) mL 50% sodium
hydroxide (Reagent 5) to approximately 900 (450) mL of water in a 1 (0.5) L
volumetric flask. Dilute to the mark and mix by inverting. Store in a plastic
bottle. Degas with helium.
By Weight: To a tared plastic 1 L container add 982 g water and 19.8 g 50%
sodium hydroxide (Reagent 5). Shake or stir to mix. Degas with helium.
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Reagent 7. Buffered EDTA (for cleaning the manifold) (RC 637)
By Volume: To a 1 (0.5) L volumetric flask add 6.75 (3.375) g ammonium
chloride (NH4Cl) and approximately 500 (250) mL water. Add 57 (28.5) mL
concentrated ammonium hydroxide (CAUTION: Fumes!) and 40.0 (20) g
tetrasodium EDTA dehydrate. Dissolve by swirling. Dilute to the mark and
mix by inverting.
By Weight: To a tared 1 L container add 6.75 g ammonium chloride (NH4Cl)
and 912 g water. Add 51.3 g concentrated ammonium hydroxide (CAUTION:
Fumes!) and 40.0 g tetrasodium EDTA dehydrate. Shake or stir to dissolve.
NOTES:
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18
QuikChem® Method 10-116-10-2-C
DETERMINATION OF SULFATE (METHYLTHYMOL BLUE) IN WATERS BY
FLOW INJECTION ANALYSIS COLORIMETRY
12 December 2000
List of Raw Materials
Ammonium Chloride (NH4Cl) – CAS 12125-02-9, (DC 675)
Ammonium Hydroxide (NH4OH) – CAS 1336-21-6, (BC 675)
Barium Chloride Dehydrate (BaCl2·2H2O) – CAS #, ( )
Ethanol (CH5OH) – CAS #, ( )
Hydrochloric Acid (HCl) – CAS 7647-01-0, (AC 675)
methylthymol blue {3,3’-bis[N,N-di(carboxymethyl)aminomethyl]-thymolsulfonephthalein, pentasodium salt} (Lachat Part no. 50243, see System Note 11.3.4) –
CAS #, (DC 675)
Sodium Hydroxide (NaOH) – CAS 1310-73-2, (BC 675)
Tetrasodium EDTA Dehydrate (Na4EDTA) – CAS #, ( )
Reagent 1. Carrier, 0.30 mg SO42-/L (RC 637)
By Volume: To a 1 L volumetric flask add 0.30 mL of 1000 mg/L Stock Sulfate
Solution (Standard 1, found in Standards Preparations section). Dilute to the
mark and mix by inverting. Degas with helium.
By Weight: To a tared 1 L container add 0.30 g of 1000 mg/L Stock Sulfate
Solution (Standard 1, found in Standards Preparation section) and 996 g water.
Shake or stir to mix. Degas with helium.
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Reagent 2. Barium Chloride Solution, 6.24 mM (RC 637)
By Volume: In a 1 L volumetric flask, dissolve 1.526 g barium chloride
dehydrate (BaCl2·2H2O) and 500 mL water. Dilute to the mark and mix by
inversion. Degas with helium.
By Weight: In a 1 L volumetric flask, dissolve 1.526 g barium chloride
dehydrate (BaCl2·2H2O) and 995 g water. Shake or stir until dissolved. Degas
with helium.
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19
Reagent 3. Hydrochloric Acid, 1.0 M
By Volume: In a 1 L volumetric flask add approximately 800 mL water and 83
mL concentrated hydrochloric acid (specific gravity 1.20, 37%). CAUTION:
Fumes! Dilute to the mark and mix by inversion. Degas with helium.
By Weight: To a tared 1 L container add 913 g water and 99.6 g concentrated
hydrochloric acid (specific gravity 1.20, 37%). CAUTION: Fumes! Shake or
stir to mix well. Degas with helium.
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Reagent 4. Barium – MTB Color Reagent
Make at least 1 Day Before Run
Note: In preparing this reagent, we have found that the purity of the
methylthymol blue and the denaturants in the alcohol are critical. USE THE
SOURCES SPECIFIED BELOW, or test the material from alternate sources for
suitability before using.
By Volume: Into a dry 500 mL volumetric flask place 0.118 g methylthymol
blue {3,3’-bis[N,N-di(carboxymethyl)aminomethyl]-thymol-sulfonephthalein,
pentasodium salt} (Lachat Part no. 50243, see System Note 11.3.4). Add 25 mL
Barium Chloride Solution (Reagent 2) which may be used to aid in the transfer
of the dye. Swirl to dissolve. Using a 5 mL Mohr pipet or a 4.0 mL volumetric
pipet, add 4.0 mL of the 1.0 M Hydrochloric Acid Solution (Reagent 3) and
mix. The solution should turn orange. Add 71 mL water and dilute to the mark
with ethanol (ethyl alcohol, specially denatured anhydrous alcohol, Aldrich
24,511-9). Mix by inverting. The pH of this solution should be 2.5. Prepare this
solution the day before use and store it refrigerated in a brown plastic bottle.
Allow to warm to room temperature before using, then degas with helium. This is
good for one week.
By Weight: To a tared 500 mL dry brown plastic bottle, place 0.118 g
methylthymol blue {3,3’-bis[N,N-di(carboxymethyl)aminomethyl]-thymolsulfonephthalein, pentasodium salt}(Lachat Part no. 50243, see System Note
11.3.4). Add 25 g Barium Chloride Solution (Reagent 2) which may be used to
aid in the transfer of the dye. Swirl to dissolve. Add 4.0 g of the 1.0 M
Hydrochloric Acid Solution (Reagent 3) and mix. The solution should turn
orange. Add 71 g water and 321 g ethanol (ethyl alcohol, specially denatured
anhydrous alcohol, Aldrich 24,511-9). Stir or shake to mix well. The pH of this
solution should be 2.5. Prepare this solution the day before use and store it
refrigerated in a brown plastic bottle. Allow to warm to room temperature before
using, then degas with helium.
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20
Reagent 5. Stock Sodium Hydroxide, 50% Solution
By Volume: In a 1 L volumetric flask, cautiously dissolve 500.0 g sodium
hydroxide (NaOH) in about 800 mL water. CAUTION: The solution will get
very hot! Cool to ambient. Dilute to the mark and mix by inversion. Store in a
plastic bottle.
By Weight: To a tared glass 1 L container add 880 g water and 500.0 g sodium
hydroxide (NaOH). CAUTION: The solution will get very hot! Shake or stir
until dissolved. Cool to ambient. Store in a plastic bottle.
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Reagent 6. Working Sodium Hydroxide , 0.18 M (RC 637)
By Volume: Using a 25 mL graduated cylinder add 14.4 mL 50% Stock
Sodium Hydroxide (Reagent 5) to approximately 900 mL of water in a 1 L
volumetric flask. Dilute to the mark and mix by inverting. Store in a plastic
bottle. Degas with helium.
By Weight: To a tared plastic 1 L container add 982 g water and 19.8 g 50%
Stock Sodium Hydroxide (Reagent 5). Shake or stir to mix. Degas with helium.
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Reagent 7. Buffered EDTA (for cleaning the manifold) (RC 637)
By Volume: To a 1 (0.5) L volumetric flask add 6.75 (3.375) g ammonium
chloride (NH4Cl) and approximately 500 (250) mL water. Add 57 (28.5) mL
concentrated ammonium hydroxide (CAUTION: Fumes!) and 40.0 (20) g
tetrasodium EDTA dehydrate. Dissolve by swirling. Dilute to the mark and
mix by inverting.
By Weight: To a tared 1 L container add 6.75 g ammonium chloride (NH4Cl)
and 912 g water. Add 51.3 g concentrated ammonium hydroxide (CAUTION:
Fumes!) and 40.0 g tetrasodium EDTA dehydrate. Shake or stir to dissolve.
NOTES:
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21
QuikChem® METHOD 10-107-04-3-A
DETERMINATION OF TOTAL NITROGEN IN WATERS BY IN-LINE
DIGESTION FOLLOWED BY FLOW INJECTION ANALYSIS
6 March 1998
List of Raw Materials
Ammonium Hydroxide (NH4OH) – CAS 1336-21-6, (BC 675)
Disodium EDTA (Na2EDTA) – CAS 6381-92-6, (DC 675)
Disodium Tetraborate Decahydrate (Sodium Borate) (Na2B4O7·10H2O) – CAS 1303-96-4,
(DC 675)
Hydrochloric Acid (HCl) – CAS 7647-01-0, (AC 675)
Sodium Metabisulphite (Na2S2O5) – CAS #, (DC 675)
N-(1-Naphthyl) Ethylenediamine Dihydrochloride (NED) – CAS 1465-25-4, (DC 675)
Phosphoric Acid (H3PO4) – CAS 7664-38-2, (AC 675)
Potassium Persulfate (K2S2O8) – CAS 7727-21-1, (DC 675)
Sodium Hydroxide (NaOH) – CAS 1310-73-2, (BC 675)
Sulfanilamide – CAS 63-74-1, (DC 675)
Sulfuric Acid (H2SO4) – CAS 7664-93-9, (AC 675)
Reagent 1. Ammonium Chloride buffer, pH 8.5
By Volume: CAUTION: Fumes!!! In a hood, to a 1 (0.5) L volumetric flask,
add 500 (250) mL water, 105 (52.5) mL concentrated hydrochloric acid (HCl),
95 (47.5)mL ammonium hydroxide (NH4OH), and 1.0 (0.5) g disodium EDTA.
Dissolve and dilute to the mark. Invert to mix. Adjust the pH to 8.5 with HCl or
15 N NaOH solution.
By Volume x2:
1000 mL H2O
210 mL HCl
100 mL rinse H2O
190 mL NH4OH
100 mL rinse H2O
1600 mL
400 mL H2O (Add 2 g EDTA to this solution)
2000 mL NH4Cl Buffer
By Weight: CAUTION: Fumes!!! In a hood, to a tared 1 L container, add 800
g water, 126 g concentrated hydrochloric acid (HCl), 85 g ammonium
hydroxide (NH4OH) and 1.0 g disodium EDTA. Stir until dissolved. Adjust the
pH to 8.5 with HCl or 15 N NaOH.
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22
Reagent 2. Sulfanilamide Color Reagent
By Volume: To a 1 L volumetric flask add about 600 (300) mL DI water. Then
add 100 (50) mL 85% phosphoric acid (H3PO4), 40.0 (20) g sulfanilamide and
1.0 (0.5) g N-(1-naphthyl)-ethylenediamine dihydrochloride (NED). Shake to
wet and stir to dissolve for 30 minutes. Dilute to the mark and invert to mix.
Store in a dark bottle and discard when the solution turns pink.
By Weight: To a tared, dark 1 L container add 876 g DI water, 170 g 85%
phosphoric acid (H3PO4), 40.0 g sulfanilamide and 1.0 g N-(1-naphtyl)
ethylenediamine dihydrochloride (NED). Shake until wetted and stir with a stir
bar for 30 minutes until dissolved. Store in a dark bottle and discard when the
solution turns pink.
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Reagent 3. Persulfate and Borate (RC 637)
NOTE: Uses largest quantity of this reagent.
By Volume: In a 1 L volumetric flask containing approximately 900 (450) mL
water, add 10 (5) g potassium persulfate (K2S2O8). The reagent from EM
Science, catalog no. PX1560-1, has been found to contain less nitrogen than other
suppliers. Add 8.75 (4.375) g disodium tetraborate decahydrate
(Na2B4O7·10H2O). Add a magnetic stirbar, dissolve and dilute to the mark. Place
in a warm water bath while stirring to aid in dissolving. Prepare weekly.
By Weight: To a tared 1 L container, add 993 g water and 10 g potassium
persulfate (K2S2O8). The reagent, from EM Science, catalog no. PX1560-1, has
been found to contain less nitrogen than from other vendors. Add 8.75 g
disodium tetraborate decahydrate (Na2B4O7·10H2O). Add a magnetic stirbar,
dissolve and dilute to the mark. Place in a warm water bath while stirring to aid
in dissolving. Prepare weekly.
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23
Reagent 4. Metabisulphite (RC 637)
By Volume: In a 1 L volumetric flask containing approximately 900 (450) mL
water, add 2.5 (1.25) g metabisulphite (Na2S2O5) from Aldrich, catalog no. 25,
555-6. Add a magnetic stirbar, dissolve and dilute to the mark. Invert to mix.
Prepare weekly.
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Reagent 5. 1.5 ml/L Sulfuric Acid
NOTE: To be used as carrier only if samples are acid preserved.
By Weight: To a tared 4 L container add about 3994 g DI water and then add 6
ml (11 g) sulfuric acid (H2SO4) and mix.
NOTES:
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24
QuikChem® METHOD 10-115-01-3-C
DETERMINATION OF TOTAL PHOSPHORUS BY FIA COLORIMETRY (INLINE PERSULFATE DIGESTION METHOD)
28 December 1998
List of Raw Materials
Ammonium Molybdate Tetrahydrate [(NH4)6Mo7O24·4H2O] – CAS 12054-85-2, (DC 675)
Antimony Potassium Tartrate (potassium antimonyl tartrate hemihydrate
K(SbO)C4H4O6·1/2 H2O) – CAS #, ( )
Antimony Potassium Tartrate (potassium antimonyl tartrate trihydrate
K(SbO)C4H4O6·3H2O) – CAS #, ( )
Ascorbic Acid (granular) – CAS 50-81-7, (DC 675)
Potassium Persulfate (K2S2O8, EM Science catalog no. PX 1560-1) – CAS 7727-21-1, (DC)
Sodium Chloride (NaCl) – CAS 7647-14-5, (DC 675)
Sodium Dodecyl Sulfate (SDS, Aldrich catalog no. 86,201-0) – CAS 151-21-3, (DC 675)
Sodium Hydroxide (NaOH) – CAS 1310-73-2, (BC 675)
Sulfuric Acid (H2SO4) – CAS 7664-93-9, (AC 675)
Reagent 1. Stock Ammonium Molybdate Solution
By Volume: In a 1 L volumetric flask dissolve 40.0 g ammonium molybdate
tetrahydrate [(NH4) 6Mo7O24·4H2O] in approximately 800 mL water. Dilute to
the mark and mix with a magnetic stirrer for at least four hours. The solution can
be stored in plastic for up to two months if refrigerated.
By Weight: To a tared 1 L container add 40.0 g ammonium molybdate
tetrahydrate [(NH4) 6Mo7O24·4H2O] and 983 g water. Mix with a magnetic
stirrer for at least four hours. The solution can be stored in plastic for up to two
months if refrigerated.
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Reagent 2. Stock Antimony Potassium Tartrate Solution
By Volume: In a 1 L volumetric flask, dissolve 3.22 g antimony potassium
tartrate (potassium antimonyl tartrate trihydrate K(SbO)C4H4O6·3H2O) or
dissolve 3.0 g antimony potassium tartrate (potassium antimonyl tartrate
hemihydrate K(SbO)C4H4O6·1/2 H2O) in approximately 800 mL water. Dilute
to the mark and mix with a magnetic stirrer until dissolved. The solution can be
stored in dark plastic for up to two months if refrigerated.
25
By Weight: To a 1 L dark, tared container add 3.22 g antimony potassium
tartrate (potassium antimonyl tartrate trihydrate K(SbO)C4H4O6·3H2O) or
dissolve 3.0 g antimony potassium tartrate (potassium antimonyl tartrate
hemihydrate) K(SbO)C4H4O6 ·1/2H2O) and 995 g water. Mix with a magnetic
stirrer until dissolved. The solution can be stored in dark plastic for up to two
months if refrigerated.
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Reagent 3. Molybdate Color Reagent (RC 637)
By Volume: To a 1 (0.5) [0.25] L volumetric flask add about 500 (250) [125]
mL water and 213 (106.5) [53.25] mL Ammonium Molybdate Solution
(Reagent 1) and 72 (36) [18] mL Antimony Potassium Tartrate Solution
(Reagent 2). Add 22.8 (11.4) [5.7] g sodium hydroxide (NaOH). Dilute to the
mark and invert to mix. Degas with helium. Prepare weekly.
By Weight: To a tared 1 L container add 715 g water and 213 g Ammonium
Molybdate Solution (Reagent 1) and 72.0 g Antimony Potassium Tartrate
Solution (Reagent 2). Add 22.8 g sodium hydroxide (NaOH). Shake and degas
with helium. Prepare weekly.
*Start at 125: 53.75mL to 250mL
*Start at 250: 107.5mL to 500mL
*Start at 500: 215mL to 1000mL - 8/2/04, anonymous
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Reagent 4. Ascorbic Acid Reducing Solution
By Volume: In a 250 (500) mL volumetric flask dissolve 17.5 (35.0) g granular
ascorbic acid in about 175 (350) mL water. Dilute to the mark and mix with a
magnetic stirrer. Degas solution with helium. Add 0.25 (0.5) g SDS (sodium
dodecyl sulfate, Aldrich catalog no. 86,201-0 or equivalent). Mix with a magnetic
stirrer. Prepare fresh every two days. Discard if the solution turns yellow.
26
By Weight: To a tared 250 (500) mL container, add 17.5 (35.0) g granular
ascorbic acid and 243.75 (487.5) g water. Mix with a magnetic stirrer until
dissolved. Degas solution with helium. Add 0.25 (0.5) g SDS (sodium dodecyl
sulfate, Aldrich catalog no. 86,201-0 or equivalent). Mix with a magnetic stirrer.
Prepare fresh every two days. Discard if the solution turns yellow.
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Reagent 5. Sulfuric Acid carrier solution (0.72 M)
By Volume: In a 1 L volumetric flask add 40 mL sulfuric acid (H2SO4) in about
600 mL water. Dilute to the mark and mix. Degas this solution with helium
after the solution is cooled down. Add 5 g sodium chloride (NaCl). Add 1.0 g
SDS (sodium dodecyl sulfate, Aldrich catalog no. 86,201-0). Invert to mix.
Prepare weekly.
By Weight: To a tared 1 L container, add 73.6 g sulfuric acid (H2SO4) into 960
g water. Degas solution with helium after the solution has cooled down. Add 5 g
sodium chloride (NaCl). Add 1.0 g SDS (sodium dodecyl sulfate, Aldrich
catalog no. 86,201-0). Invert to mix. Prepare weekly.
For 2 L Sulfuric Acid Carrier
1000 mL H2O
80 mL H2SO4
100 mL H20 Rinse
10 g NaCl
2 g SDS
1180 mL Total
820 mL H2O
2L
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PREPARATION OF DIGESTION REAGENTS
Reagent 6. Digestion Reagent 1
By Volume: In a 1 (0.5) L volumetric flask add 500 (250) mL DI water and
106.5 (53.25) mL sulfuric acid (H2SO4). Dilute to the mark and invert to mix.
(CAUTION: This solution will become very hot!) Prepare weekly. Carefully
degas before using.
27
By Weight: To a tared 1 L container add 893.5 g DI water and 196.0 g sulfuric
acid (H2SO4). (CAUTION: This solution will become very hot!) Prepare
weekly. Carefully degas before using.
*Add 196.75 mL DI water to the solution of 250 mL DI water + 53.25 mL
sulfuric acid in order to dilute to 500 mL. -8/2/04, anonymous
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Reagent 7. Digestion Reagent 2
By Volume: In a 500 mL volumetric flask add 250 mL DI water and 13 g
potassium persulfate (K2S2O8, EM Science catalog no. PX 1560-1). Mix with a
magnetic stirrer until dissolved. Prepare weekly. Degas before using.
By Weight: In a 1 L volumetric flask add 500 mL DI water and 26 g potassium
persulfate (K2S2O8, EM Science catalog no. PX 1560-1). Mix with a magnetic
stirrer until dissolved. Prepare weekly. Degas before using.
NOTES:
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28