Solids, Total Volatile and Fixed, 8276

Solids, Total Volatile and Fixed DOC316.53.001205

Gravimetric Method1 Method 8276

Scope and Application: For potable, surface and saline water and domestic and industrial wastewater.
1 Adapted from Standard Methods for the Examination of Water and Wastewater.

Test preparation

Before starting the test:

When measuring volatile solids, ignite the aluminum dishes for one hour at 550 °C prior to use.

Larger sample sizes may be used. For larger samples, use an evaporating dish and a steam bath to evaporate the liquid.

Samples from Method 8271 may be used directly in this procedure. Use the resulting sample and start this method at step 7.

Collect the following items:

Description Quantity

Weighing dish, aluminum 1

Drying oven 1

Graduated cylinder, 50 mL 1

Desiccator and desiccant 1

Analytical balance 1

Muffle furnace 1

See Consumables and replacement items for reorder information.

Solids, Total Volatile and Fixed

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Solids, Total Volatile and Fixed

Gravimetric Method

1. Heat an aluminum 1. Weigh an aluminum 2. Mix the sample and 3. Place the sample in a
dish to 550 °C for one dish to the nearest 0.1 mg add 50 mL to the preheated oven and
hour. Store and cool the (0.0001 g). Record this mg aluminum dish. Use a evaporate at 103–105 °C
dish in a desiccator until value as C. blender or a beaker with for approximately six
needed. stir bar and stir plate to mix hours.
If a sample from Method the samples. Highly mineralized water
8271 is used, omit steps may prolong the drying
2–6. Proceed to step 7. time.
Note: A steam bath and
evaporating dish may be
used in place of the drying
oven for larger samples.
After evaporation on the
steam bath, dry the dish to
constant weight in a
103–105 °C drying oven.

4. Take the dish out of 5. Weigh the dish to the 6. Transfer the aluminum 7. Weigh the dish to the
the oven and allow it to nearest 0.1 mg (0.0001 g) dish into a pre-heated nearest 0.1 mg using an
cool to room temperature using an analytical muffle furnace at 550 °C analytical balance.
in a desiccator. balance. Record this mg for 30 minutes. Repeat ignition until two
value as A. After 30 minutes, take the successive sample
dish out of the furnace with weighings (A – B) do not
tongs and cool to room differ by more than 4% or
temperature in a 0.5 mg, whichever is less.
desiccator. Record this mg value as B.

Solids, Total Volatile and Fixed

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 Solids, Total Volatile and Fixed

Gravimetric Method (continued)

8. The loss of weight is

total volatile solids.
Weighed residue is total
fixed solids.
Calculate:
mg/L Volatile Solids
( A – B ) × 1000
= ---------------------------------------------------------------
sample in volume in mL

mg/L Fixed Solids

( B – C ) × 1000
= --------------------------------------------------------
sample volume in mL

where:
A = Weight (mg) of solids
+ dish before ignition at
550 °C
B = Weight (mg) of solids
+ dish after ignition at
550 °C
C = Weight (mg) of empty
dish

Sample collection, preservation and storage

• Collect samples in clean plastic or glass bottles.
• Samples should be analyzed as soon as possible after collection, but can be stored up to
seven days by cooling to 4 °C (39 °F).

Summary of method
A well-mixed sample is evaporated in a weighed dish and dried to a constant weight in a
103–105 °C oven. The dish and sample are ignited at 550 °C for 30 minutes. The loss of sample
mass upon ignition represents the volatile solids. The remaining sample after ignition represents
the fixed solids.

Solids, Total Volatile and Fixed

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Solids, Total Volatile and Fixed

Consumables and replacement items

Required apparatus
Description Unit Catalog number
Balance, Analytical, 115 VAC, 60 Hz each 2936701
Cylinder, graduated, 50 mL each 50841
Desiccant, indicating Drierite each 2088701
Desiccator, without stopcock each 1428500
Desiccator Plate, ceramic each 1428400
Dish, aluminum (63 x 17.5 mm) 100/pkg 2164000
Furnace, muffle, 120 Vac, 50/60 Hz each 1429600
Furnace, muffle, 240 Vac, 50/60 Hz each 1429624
Oven, laboratory, 240 Vac, 50 Hz each 1428902
Water, deionized 4L 27256
Oven, laboratory, 120 VAC, 60 Hz each 1428900
Tongs each 56900

Optional reagents and apparatus

Description Unit Catalog number
Blender, 1.2 liter, 120 VAC each 2616100
Blender, 1.2 liter, 240 VAC each 2616102
Stirrer, Magnetic, 4 x 4, 115 VAC each 2881200
Stirrer, magnetic, 4 x 4, 230 VAC each 2881202
Beaker, Glass, 250 mL each 50046H
Stir Bar, 22 x 8 mm each 2095350
Steam Bath, 8 inch diameter each 2347900
Evaporating Dish, porcelain, 120 mL each 52561
Bottles, w/cap, wide mouth, 500 mL poly 12/pkg 2087079

FOR TECHNICAL ASSISTANCE, PRICE INFORMATION AND ORDERING: HACH COMPANY

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© Hach Company, 2007. All rights reserved. Printed in the U.S.A. Updated February 2008, Edition 5