Police officers behind riot shields hurled smoke grenades at dozens of protesters to enforce a citywide curfew, imposed after the worst outbreak of rioting in Baltimore since 1968.
Demonstrators threw bottles at police, and picked up the smoke canisters and hurled them back at officers.
No immediate arrests or serious injuries were reported, and the crowd rapidly dispersed. It was down to just a few dozen people within minutes.
The clash came after a day of high tension but relative peace in Baltimore, as thousands of police officers and National Guardsmen poured into the city to prevent another round of rioting like the one that rocked the city on Monday.
It was the first time since the assassination of the Rev Martin Luther King Jr in 1968 that the National Guard was called out in Baltimore to prevent civil unrest.
Maryland's governor said 2,000 Guardsmen and 1,000 law officers would be in place overnight.
"This combined force will not tolerate violence or looting," Governor Larry Hogan warned.
The racially charged violence on Monday was set off by the case of Freddie Gray, a 25-year-old black man who died of a spinal-cord injury under mysterious circumstances while in police custody.
In a measure of how tense things were, Baltimore was under a citywide 10pm to 5am emergency curfew.
All schools were closed, and the Baltimore Orioles cancelled last night's game at Camden Yards and - in what may be a first in baseball's 145-year history - announced today's match will be closed to the public.
The streets were largely calm all day and into the evening, with only a few scattered arrests. The real test was expected after dark.
As the curfew went into effect, several hundred protesters remained in the street in the city's Penn North section near where a pharmacy was looted.
Standing shoulder to shoulder, police in helmets and riot shields began advancing toward the demonstrators in an effort to push them back. Some protesters lay in the street or hurled bottles toward the police.
As the hour drew near, a local pastor used a loudspeaker to urge the demonstrators to go home, saying: "Let's show the world, because the eyes of the world are on Baltimore right now."
Around the same time and in a different neighbourhood, police tweeted that they were making arrests in South Baltimore after people started attacking officers with rocks and bricks. At least one officer was reported injured.
Monday's looting, arson and rock- and bottle-throwing by mostly black rioters broke out just hours after Mr Gray's funeral
Political leaders and residents called the violence a tragedy for the city and lamented the damage done by the rioters to their own neighbourhoods.
"I had officers come up to me and say, 'I was born and raised in this city. This makes me cry,'" Baltimore Police Commissioner Anthony Batts said.
Haywood McMorris, manager of the wrecked pharmacy, said the destruction did not make sense: "We work here, man. This is where we stand, and this is where people actually make a living."
But the rioting also brought out a sense of civic pride and responsibility in many Baltimore residents, with hundreds of volunteers turning out to sweep the streets of glass and other debris with brooms and rubbish bags donated by hardware stores.
At the White House, President Barack Obama called the deaths of several black men around the country at the hands of police "a slow-rolling crisis".
But he added there was "no excuse" for the violence in Baltimore, and said the rioters should be treated as criminals.
"They aren't protesting. They aren't making a statement. They're stealing," Mr Obama said.
The rioting started in West Baltimore on Monday afternoon and by midnight had spread to East Baltimore and neighbourhoods close to the city centre.
At least 20 officers were hurt, one person was critically injured in a fire, more than 200 adults and 34 juveniles were arrested, and nearly 150 cars were burned, police said. The governor had no immediate estimate of the damage.
In the aftermath of the riots, state and local authorities found themselves facing questions about whether they let things spin out of control.
Mr Batts said police did not move in faster because those involved in the early stages were just "kids" - teenagers who had just been let out of school.
Mayor Stephanie Rawlings-Blake waited hours to ask the governor to declare a state of emergency, and the governor hinted she should have come to him earlier.
Ms Rawlings-Blake said officials initially thought they had the unrest under control.
Mr Gray was arrested on April 12 after running away at the sight of police, authorities said.
He was held down, handcuffed and loaded into a police van. Leg cuffs were put on him when he became angry inside. He died a week later.
Authorities said they are still investigating how and when he suffered the spinal injury - during the arrest or while he was in the van, where he was riding without being belted in, a violation of department policy.
Six officers have been suspended with pay in the meantime.